Sample records for active voltammetric microsensors

Many industrial and environmental processes, including bioremediation, would benefit from the feedback and control information provided by a local multi-analyte chemical sensor. For most processes, such a sensor would need to be rugged enough to be placed in situ for long-term remote monitoring, and inexpensive enough to be fielded in useful numbers. The multi-analyte capability is difficult to obtain from common passive sensors, but can be provided by an active device that produces a spectrum-type response. Such new active gas microsensor technology has been developed at Argonne National Laboratory. The technology couples an electrocatalytic ceramic-metallic (cermet) microsensor with a voltammetric measurement technique and advanced neural signal processing. It has been demonstrated to be flexible, rugged, and very economical to produce and deploy. Both narrow interest detectors and wide spectrum instruments have been developed around this technology. Much of this technology's strength lies in the active measurement technique employed. The technique involves applying voltammetry to a miniature electrocatalytic cell to produce unique chemical ''signatures'' from the analytes. These signatures are processed with neural pattern recognition algorithms to identify and quantify the components in the analyte. The neural signal processing allows for innovative sampling and analysis strategies to be employed with the microsensor. In most situations, the whole response signature from the voltammogram can be used to identify, classify, and quantify an analyte, without dissecting it into component parts. This allows an instrument to be calibrated once for a specific gas or mixture of gases by simple exposure to a multi-component standard rather than by a series of individual gases. The sampled unknown analytes can vary in composition or in concentration, the calibration, sensing, and processing methods of these activevoltammetricmicrosensors can detect, recognize, and

Microsensors used in microbial ecology are reviewed with emphasis on new sensor developments (NO3-, NO2-, NH4+, CO2, H2, H2S and CH4 microsensors as well as fiberoptical microsensors for O2, temperature and pH). Examples of microsensor applications in biofilms and activated sludge flocs are presented, in which sulfate reduction and denitrification were studied. PMID:10022061

Phototrophic biofilms are widely distributed in nature and their ecological importance is well recognized. More recently, there has been a growing interest in using artificial phototrophic biofilms in innovative photobioreactors for production of microalgal biomass in biotechnological applications. To study physiological processes within these biofilms, microsensors have been applied in several studies. Here, the 'light-dark shift method' relies on measurement of photosynthetic activity in terms of light-induced oxygen production. However, when applied to non-submerged biofilms that can be found in numerous locations in nature, as well as in some types of photobioreactors, limitations of this approach are obvious due to rapid removal of gaseous species at the biofilm surface. Here, we introduce a mathematical correction to recover the distribution of the actual photosynthetic activity along the depth gradient in the biofilm, based on a numerical solution of the inversed diffusion equation of oxygen. This method considers changes in mass transport during the measurement period as can found on biofilms possessing a thin flow/mass transfer boundary layer (e. g., non-submerged biofilms). Using both simulated and real microsensor data, the proposed method was shown to be much more accurate than the classical method, which leads to underestimations of rates near the biofilm surface. All test profiles could be recovered with a high fit. According to our simulated microsensor measurements, a depth resolution of ≤20 μm is recommended near the surface. We conclude that our method strongly improves the quality of data acquired from light-dark measurements of photosynthetic activity in biofilms. PMID:26232709

This video looks at a spinoff application of the technology from advanced microsensors -- those that monitor and determine conditions of spacecraft like the Space Shuttle. The application featured is concerned with the monitoring of the health of premature babies.

Eugenia dysenterica DC (cagaiteira) is a native tree from Cerrado biome. Cagaita fruits are known and consumed in natura, mainly by inhabitants from Cerrado. In this study, we evaluated the antioxidant activity of leaves of this plant. For this evaluation we used four methods, the reduction of phosphomolybdenum, scanning by hydrogen peroxide, DPPH radical scavenging assay and determination of electrochemical parameters by differential pulse voltammetry. The results indicate that all extracts from leaves of this species have significant antioxidant potential, following the order: crude ethanol extract CEE) >crude aqueous extract (CAE) >crude hexane extract (CHE). The voltammetric approaches were also applied in order to evaluate the redox behavior of the hydrophilic extracts, as well as of their sub-extracts. Thus, the results suggest the presence of catechol-like polyphenols, which were confirmed by chromatography and phytochemical methods. Voltammetric analysis showed to be a reliable and fast method to determine redox behavior of E. dysenterica extracts. PMID:27087097

This paper describes the construction of 2 microsensor units for on-line voltammetric detection inside a cylindrical microcell (a working microsensor unit and a reference and auxiliary microsensor unit), for application to heavy-metal analysis in complex media such as natural waters. Both microsensor units include a channel for the solution renewal in the microcell after analysis. The working microsensor, a Hg-plated Ir microelectrode, is protected against fouling with an agarose gel including a hydrophobic chromatographic phase (C18). The fabrication steps and the quality tests related to long-term use and reliability, as well as to precision, are described. The application of the protective gel layer against fouling by hydrophobic or surface active small molecules is of general application, reliable, and very efficient. The reference and auxiliary unit is composed by an iridium oxide based mini reference electrode, an auxiliary Pt electrode, and a circulation channel. It is built to enable its use inside a 700-microm-diameter tubing connected to a hollow fiber supported liquid membrane lumen (volume, 5-10 microL) for heavy-metal analysis. However, it can be used in any other microanalytical system. The reference electrode is sufficiently stable for voltammetric applications (1-2 mV drift/day), and its lifetime is more than one year. The Ti/IrO2 core is immersed in a pH-buffered agarose gel, to guarantee potential stability even when the electrode is immersed in variable pH solutions. PMID:10739195

We report on a plasticized polyurethane ionophore-based thin film material (of hundreds of nanometer thickness) for simultaneous voltammetric multianalyte ion activity detection triggered by the oxidation/reduction of an underlying poly(3-octylthiophene) film. This material provides excellent mechanical, physical, and chemical robustness compared to other polymers. Polyurethane films did not exhibit leaching of lipophilic additives after rinsing with a direct water jet and exhibited resistance to detachment from the underlying electrode surface, resulting in a voltammetric current response with less than <1.5% RSD variation (n = 50). In contrast, plasticized poly(vinyl chloride), polystyrene, and poly(acrylate) ionophore-based membranes of the same thickness and composition exhibited a significant deterioration of the signal after identical treatment. While previously reported works emphasized fundamental advancement of multi-ion detection with multi-ionophore-based thin films, polyurethane thin membranes allow one to achieve real world measurements without sacrificing analytical performance. Indeed, polyurethane membranes are demonstrated to be useful for the simultaneous determination of potassium and lithium in undiluted human serum and blood with attractive precision. PMID:27187779

The effect of uranium added in ecologically relevant concentrations (1 × 10 -5 and 1 × 10 -6 M) to stable multispecies biofilms was studied by electrochemical oxygen microsensors with tip diameters of 10 μm and by confocal laser fluorescence microscopy (CLSM). The microsensor profile measurements in the stable multispecies biofilms exposed to uranium showed that the oxygen concentration decreased faster with increasing biofilm depth compared to the uranium free biofilms. In the uranium containing biofilms, the oxygen consumption, calculated from the steady-state microprofiles, showed high consumption rates of up to 61.7 nmol cm -3 s -1 in the top layer (0-70 μm) and much lower consumption rates in the lower zone of the biofilms. Staining experiments with 5-cyano-2,3-ditolyl tetrazolium chloride (CTC) and 4,6-diamidino-2-phenylindole (DAPI) confirmed the high respiratory activities of the bacteria in the upper layer. Analysis of the amplified 16S rRNA gene fragments showed that the addition of uranium in ecologically relevant concentrations did not change the bacterial diversity in the stable multispecies biofilms and is therefore not responsible for the different oxygen profiles in the biofilms. The fast decrease in the oxygen concentrations in the biofilm profiles showed that the bacteria in the top region of the biofilms, i.e., the metabolically most active biofilm zone, battle the toxic effects of aqueous uranium with an increased respiratory activity. This increased respiratory activity results in O 2 depleted zones closer to the biofilm/air interface which may trigger uranium redox processes, since suitable redox partners, e.g., extracellular polymeric substance (EPS) and other organics (e.g., metabolites), are sufficiently available in the biofilm porewaters. Such redox reactions may lead to precipitation of uranium (IV) solids and consequently to a removal of uranium from the aqueous phase.

Sandia National Laboratories, an 8500+ person, multiprogram research and development facility operated for the US Department of Energy, has over 400 research, development and applications scientists and engineers working on sensor technologies. Sandia`s 20 person Microsensors Research and Development Department has invented, developed and fielded sensor systems based on acoustic, fiber optic, and silicon microelectronic technologies. These sensors have been used for diverse applications inducting the monitoring of cleaning chemical concentrations in industrial process effluent streams, detection of explosive gas concentrations in aging industrial equipment, real-time measurements of fluid viscosity in equipment lubricants, and monitoring of contaminant concentration levels in ultrapure process gases. Representative sensor technologies available for technology transfer will be described including bulk acoustic wave resonators, surface acoustic wave devices, fiber optic micromirror sensors, and silicon microelectronic sensors.

As shown in recent work, thin layer ion-selective multi-ionophore membranes can be interrogated by cyclic voltammetry to detect the ion activity of multiple species simultaneously and selectively. Additional fundamental evidence is put forward on ion discrimination with thin multi-ionophore-based membranes with thicknesses of 200 ± 25 nm and backside contacted with poly-3-octylthiophene (POT). An anodic potential scan partially oxidizes the POT film (to POT(+)), thereby initiating the release of hydrophilic cations from the membrane phase to the sample solution at a characteristic potential. Varying concentration of added cation-exchanger demonstrates that it limits the ion transfer charge and not the deposited POT film. Voltammograms with multiple peaks are observed with each associated with the transfer of one type of ion (lithium, potassium, and sodium). Experimental conditions (thickness and composition of the membrane and concentration of the sample) are chosen that allow one to describe the system by a thermodynamic rather than kinetic model. As a consequence, apparent stability constants for sodium, potassium, and lithium (assuming 1:1 stoichiometry) with their respective ionophores are calculated and agree well with the values obtained by the potentiometric sandwich membrane technique. As an analytical application, a membrane containing three ionophores was used to determine lithium, sodium, and potassium in artificial samples at the same location and within a single voltammetric scan. Lithium and potassium were also determined in undiluted human plasma in the therapeutic concentration range. PMID:26712342

Microbially influenced corrosion (MIC) in concrete results in significant cost for infrastructure maintenance. Prior studies have employed molecular techniques to identify microbial community species in corroded concrete, but failed to explore bacterial activity and functionality during deterioration. In this study, biofilms of different sulfur-oxidizing bacteria compositions were developed on the surface of cement paste samples to simulate the natural ecological succession of microbial communities during MIC processes. Noninvasive, self-referencing (SR) microsensors were used to quantify real time changes of oxygen, hydrogen ion and calcium ion flux for the biofilm to provide more information about bacterial behavior during deterioration. Results showed higher transport rates in oxygen consumption, and hydrogen ion at 4 weeks than 2 weeks, indicating increased bacterial activity over time. Samples with five species biofilm had the highest hydrogen ion and calcium ion transport rates, confirming attribution of acidophilic sulfur-oxidizing microorganisms (ASOM). Differences in transport rates between three species samples and two species samples confirmed the diversity between Thiomonas intermedia and Starkeya novella. The limitations of SR sensors in corrosion application could be improved in future studies when combined with molecular techniques to identify the roles of major bacterial species in the deterioration process. PMID:26707733

The Microsensors Program was born out the need for enhanced sensor technology in support of the Weapons Program. In the interest of expanded diagnostic capabilities to provide true performance characteristics of weapon assemblies in flight and ground tests, a suite of sensor requirements was proposed. These potential new sensor technologies were envisioned to be completely unobtrusive and allow for the development of test vehicles (mock warheads and bomb assemblies) that were designed to mechanical and electrical specifications as close to the stockpile weapon design configuration as possible. The closeness of a test vehicle design to the respective stockpile weapon design is referred to as ''fidelity,'' with the term ''high-fidelity'' to mean all components are designed to emulate, very closely, the true system design. These efforts were in line with many activities associated with Stockpile Stewardship and were intended to enable better modeling and performance assessment without the need for underground testing. Several weapons are currently undergoing Life Extension Programs (LEP) to lengthen each weapon system's respective service life. The ability to assess the projected life of these complex assemblies is crucial to the success of the LEP activities.

A top concern in homeland security efforts is the lack of ability to monitor the thousands of miles of open border with our neighbors. It is not currently feasible to continually monitor the borders for illegal intrusions. The MicroSensor System (MSS) seeks to achieve a low-cost monitoring solution that can be efficiently deployed for border patrol applications. The modifications and issues regarding the unique requirements of this application will be discussed and presented. The MicroSensor System was developed by the Defense Microelectronics Activity (DMEA) for military applications, but border patrol applications, with their unique sensor requirements, demand careful adaptation and modification from the military application. Adaptation of the existing sensor design for border applications has been initiated. Coverage issues, communications needs, and other requirements need to be explored for the border patrol application. Currently, border patrol has a number of deficiencies that can be addressed with a microsensor network. First, a distributed networked sensor field could mitigate the porous border intruder detection problem. Second, a unified database needs to be available to identify aliens attempting to cross into the United States. This database needs to take unique characteristics (e.g. biometrics, fingerprints) recovered from a specialized field unit to reliably identify intruders. Finally, this sensor network needs to provide a communication ability to allow border patrol officers to have quick access to intrusion information as well as equipment tracking and voice communication. MSS already addresses the sensing portion of the solution, including detection of acoustic, infrared, magnetic, and seismic events. MSS also includes a low-power networking protocol to lengthen the battery life. In addition to current military requirements, MSS needs a solar panel solution to extend its battery life to 5 years, and an additional backbone communication link

In one general embodiment, a system includes at least one microsensor configured to detect one or more conditions of a fluidic medium of a reservoir; and a receptacle, wherein the receptacle encapsulates the at least one microsensor. In another general embodiment, a method include injecting the encapsulated at least one microsensor as recited above into a fluidic medium of a reservoir; and detecting one or more conditions of the fluidic medium of the reservoir.

Sensors have been developed and manufactured by microelectronic fabrication techniques to directly measure corrosion rates and to determine the effectiveness of corrosion control systems. Microsensors based on measurements of corrosion rate by linear polarization, electrical resistance change, and galvanic currents have been devised. Analytical measurements by potentiometric and amperometric techniques using thick-film planar transducers are illustrated. The use of generic sensor elements individually and in combination to attest the status of corrosion control and to provide data for the evaluation of future performance is highlighted.

Sulfate reducing bacteria (SRB) play significant roles in anaerobic environments in oil sands mature fine tailings (MFTs). Hydrogen sulfide (H2S) is produced during the biological sulfate reduction process. The production of toxic H2S is one of the concerns because it may hinder the landscape remediation efficiency of oil sands tailing ponds. In present study, the in situ activity and the community structure of SRB in MFT and gypsum amended MFT in two settling columns were investigated. Combined techniques of H2S microsensor and dissimilatory sulfite reductase β-subunit (dsrB) genes-based real time quantitative polymerase chain reaction (qPCR) were applied to detect the in situ H2S and the abundance of SRB. A higher diversity of SRB and more H2S were observed in gypsum amended MFT than that in MFT, indicating a higher sulfate reduction activity in gypsum amended MFT; in addition, the activity of SRB varied as depth in both MFT and gypsum amended MFT: the deeper the more H2S produced. Long-term plans for tailings management can be assessed more wisely with the information provided in this study. PMID:27266310

A sensor by definition should be non-intrusive and respond faithfully to the parameter that one is trying to measure. Ideally the sensor should be small so that it does not disturb the field it is trying to measure and permit implementation on new and existing systems without requiring redesign of the system. Power supply to activate the sensor and extract data from the sensor is often the Achilles heel in implementation. Surface Acoustic Wave (SAW) devices also called the IDT Microsensor fit the bill ideally. They are in fact the first MEMS devices made, although this is not generally recognized. Unlike other MEMS devices, a SAW device has no moving parts. SAW devices can be mass-produced using semiconductor fabrication methods. The operation and use of Inter Digital Transducer (IDT) microsensor will be reviewed. Our major interest is that these sensors operate at RF frequencies and can hence be excited wirelessly using microstrip antennas from a remote source. Thus, one can achieve a passive sensor and retrieve the sensor data wirelessly. Whenever sensing is needed on a rapidly rotating system such as helicopter blades or automobile tires, in subsurface situations or inaccessible locations, a wireless passive sensor is the ideal solution. This talk will overview research on design and application of wireless IDT microsensors to dynamical strain monitoring, ice sensing, temperature and humidity sensing, liquid characterization and currently to tire pressure measurements.

Serially diluted and agitated (SAD) drugs available commercially are in use with great faith because of the astonishing results they produce. The scientific viewpoint attached to the centuries-old therapy with SAD drugs, as in homeopathy, remained doubtful for want of appropriate research and insufficient evidence base. The conflicting points related to SAD drug mostly related to the level of concentrations/dilutions, use of drug in contradictory clinical conditions compared to the modern system of medicine, identification of medicinally active ingredient in concentrations and dilutions used in commercially available SAD drugs, and lack of laboratory-based pharmacological data vis-à-vis modern medicine. Modus operandi of SAD drug is also unknown. To address some of these issues an analytical study was carried out wherein commercially available SAD drug Digitalis purpurea, commonly used in different systems of medicine, was put to test. Various concentrations of commercially available Digitalis purpurea were analyzed using analytical methods: cyclic voltammetry, emission spectroscopy, and UV-VIS spectroscopy. These analytical methods apparently identified the medicinal ingredients and effect of serial dilution in commercial preparation of the drugs. PMID:22606641

The objectives of the Low Cost Microsensors (LCMS) Program are twofold. The first is to develop and deliver a long-range infrared (IR) sensor built upon an uncooled vanadium oxide (VOx) 640 X 512 format focal plane array (FPA) engine. The second is to develop an expendable microsensor built upon a VOx 160 X 128 format FPA engine. The 640 X 480 sensor is applicable to long-range surveillance and targeting missions and is a reusable asset. The 160 X 120 sensor is designed for applications where miniaturization is required as well as low cost and low power. The 160 X 120 is also intended for expendable military applications. The intent of this DUS&T effort is to further reduce the cost, weight, and power of uncooled IR sensors, and to increase the capability of these sensors, thereby expanding their applicability to military and commercial markets never before addressed by thermal imaging.

Numerous aerospace applications, including low-false-alarm fire detection, environmental monitoring, fuel leak detection, and engine emission monitoring, would benefit greatly from robust and low weight, cost, and power consumption chemical microsensors. NASA Glenn Research Center has been working to develop a variety of chemical microsensors with these attributes to address the aforementioned applications. Chemical microsensors using different material platforms and sensing mechanisms have been produced. Approaches using electrochemical cells, resistors, and Schottky diode platforms, combined with nano-based materials, high temperature solid electrolytes, and room temperature polymer electrolytes have been realized to enable different types of microsensors. By understanding the application needs and chemical gas species to be detected, sensing materials and unique microfabrication processes were selected and applied. The chemical microsensors were designed utilizing simple structures and the least number of microfabrication processes possible, while maintaining high yield and low cost. In this presentation, an overview of carbon dioxide (CO2), oxygen (O2), and hydrogen/hydrocarbons (H2/CxHy) microsensors and their fabrication, testing results, and applications will be described. Particular challenges associated with improving the H2/CxHy microsensor contact wire-bonding pad will be discussed. These microsensors represent our research approach and serve as major tools as we expand our sensor development toolbox. Our ultimate goal is to develop robust chemical microsensor systems for aerospace and commercial applications.

Understanding the limiting factors and mechanisms of biofilm processes requires the direct measurement of microscale gradients using the appropriate tools. Microscale measurements can provide mechanistic information that cannot be obtained from bulk-scale measurements. Among the most used and trusted tools in microscale biofilm research are microsensors. The goal of this chapter is to introduce microsensor technology along with several examples to illustrate microscale processes in biofilms that are usually absent in bulk. We define a microsensor for biofilm research as a needle-type sensor with tip diameter of a few microns and a length up to several hundred microns. Microsensors can be used noninvasively to monitor in situ biofilm processes. Both optical and electrochemical microsensors can be used for biofilm applications. Because of newly discovered biofilm processes, the design and use of microsensors require customization and carefully designed experiments. In this chapter we present several examples describing the use of microsensors (1) in environmental biofilms, (2) in medical biofilms, and (3) in biofilms for energy and bioproducts. Microsensors can be the most useful if the measured profiles are integrated into the study of overall biofilm processes. PMID:24008918

The Low Cost Microsensors (LCMS) Program recently demonstrated state-of-the-art imagery in a long-range infrared (IR) sensor built upon an uncooled vanadium oxide (VOx) 640 X 480 format focal plane array (FPA) engine. The 640 X 480 sensor is applicable to long-range surveillance and targeting missions. The intent of this DUS&T effort is to further reduce the cost, weight, and power of uncooled IR sensors, and to increase the capability of these sensors, thereby expanding their applicability to military and commercial markets never before addressed by thermal imaging.

An innovative fiber optic pressure microsensor has been developed that is based upon on Luna Innovations' patented extrinsic Fabry-Perot interferometric (EFPI) technique. The basic physics governing the operation of these sensors makes them relatively tolerant or immune to the effects of high-temperature, high-EMI, and highly-corrosive environments. Luna's pressure microsensor is extremely small, with an outer diameter of only 200 microns and a length of less than 1mm. The pressure microsensor has a high sensitivity that allows for sub-mmHg resolution over a dynamic range of 0-300 mmHg. The combination of these features makes this pressure microsensor ideal for medical applications where small size, high sensitivity and accuracy, EMI immunity, biocompatibility, and survivability (e.g. sterilizable - steam, ethylene oxide) are important. One example medical application of the pressure microsensor has been to adapt the microsensor for measurement of intramuscular pressure in vivo during active and passive muscle activation. Clinically it is difficult to study the in vivo mechanical properties of individual skeletal muscles for a variety of reasons. Initial experiments have demonstrated a correlation between intramuscular pressure and force. Such measurements can be a useful diagnostic tool for clinicians assessing muscular deficits in patients.

An integrated optical capillary electrophoresis system for analyzing an analyte. A modulated optical pump beam impinges on an capillary containing the analyte/buffer solution which is separated by electrophoresis. The thermally-induced change in the index of refraction of light in said electrophoresis capillary is monitored using an integrated micro-interferometer. The interferometer includes a first interferometer arm intersecting the electrophoresis capillary proximate the excitation beam and a second, reference interferometer arm. Changes in index of refraction in the analyte measured by interrogating the interferometer state using white light interferometry and a phase-generated carrier demodulation technique. Background thermo-optical activity in the buffer solution is cancelled by splitting the pump beam and exciting pure buffer solution in a second section of capillary where it crosses the reference arm of the interferometer.

Testing for plant experiments in space has begun to explore active nutrient delivery concepts in which water and nutrients are replenished on a continuous basis for long-term growth. The goal of this study is to develop a novel microsensor array to provide information on the dissolved oxygen environment in the plant root zone for the optimum control of hydroponics and solid substrate plant cultivation systems in the space environment. Miniaturized polarographic dissolved oxygen sensors have been designed and fabricated on a flexible Kapton (trademark) (polyimide) substrate. Two capabilities of the new microsensor array were explored. First, measurements of dissolved oxygen in the plant root zone in hydroponics and solid substrate culture systems were made. The microsensor array was fabricated on a flexible substrate, and then cut out into a mesh type to make a suspended array that could be placed either in a hydroponics system or in a solid substrate cultivation system to measure the oxygen environments. Second, the in situ self-diagnostic and self-calibration capability (two-point for oxygen) was adopted by dynamically controlling the microenvironment in close proximity to the microsensors. With a built-in generating electrode that surrounds the microsensor, two kinds of microenvironments (oxygen-saturated and oxygen-depleted phases) could be established by water electrolysis depending on the polarity of the generating electrode. The unique features of the new microsensor array (small size, multiple sensors, flexibility and self-diagnosis) can have exceptional benefits for the study and optimization of plant cultivation systems in both terrestrial and microgravity environments. The in situ self-diagnostic and self-calibration features of the microsensor array will also enable continuous verification of the operability during entire plant growth cycles. This concept of automated control of a novel chemical monitoring system will minimize crew time required for

A voltammetric membrane electrode system has been modified and applied to the in situ measurement of chlorine dioxide. The electrode system consisted of a gold cathode, a silver/silver chloride reference electrode, and a gold counter electrode. Different membrane materials were t...

The use of microsensors for in-field monitoring of environmental parameters is gaining interest due to their advantages over conventional sensors. Among them microsensors based on semiconductor technology offer additional advantages such as small size, robustness, low output impedance and rapid response. Besides, the technology used allows integration of circuitry and multiple sensors in the same substrate and accordingly they can be implemented in compact probes for particular applications e.g., in situ monitoring and/or on-line measurements. In the field of microsensors for environmental applications, Ion Selective Field Effect Transistors (ISFETs) have a special interest. They are particularly helpful for measuring pH and other ions in small volumes and they can be integrated in compact flow cells for continuous measurements. In this paper the technologies used to fabricate ISFETs and a review of the role of ISFETs in the environmental field are presented. PMID:22315527

In this article, the relation between position accuracy and the number of simultaneously measured values, such as coordinates, has been analyzed. Based on this, a conceptual layout of MEMS devices (microsensors) for multidimensional position monitoring comprising a single anchored and a single actuated part has been developed. Both parts are connected with a plurality of micromechanical flexures, and each flexure includes position detecting cantilevers. Microsensors having detecting cantilevers oriented in X and Y direction have been designed and prototyped. Experimentally measured results at characterization of 1D, 2D and 3D position microsensors are reported as well. Exploiting different flexure layouts, a travel range between 50μm and 1.8mm and sensors' sensitivity in the range between 30μV/μm and 5mV/μm@ 1V DC supply voltage have been demonstrated. A method for accurate calculation of all three Cartesian coordinates, based on measurement of at least three microsensors' signals has also been described. The analyses of experimental results prove the capability of position monitoring with ppm-(part per million) accuracy. The technology for fabrication of MEMS devices with sidewall embedded piezoresistors removes restrictions in strong improvement of their usability for position sensing with a high accuracy. The present study is, also a part of a common strategy for developing a novel MEMS-based platform for simultaneous accurate measurement of various physical values when they are transduced to a change of position.

A new voltammetric membrane electrode for trace analysis of ozone was developed. The effects of stirring and temperature as well as the response time were investigated. Using a three-electrode voltammetric cell, and a gas permeable membrane, measurements were done using steady-st...

The MicroSensors Systems (MSS) Program is developing a layered sensor network to detect dismounted threats approaching high value assets. The MSS subsystem elements include sensitive receivers (capable of detecting<<1 Watt emissions in dense signal or degraded signal environments) and low power, miniature, disposable sensors (acoustic, magnetic, and infrared). A novel network protocol has been developed to reduce the network traffic resulting in conservation of system power and lower probability of detection and interception. The MSS program will provide unprecedented levels of real-time battlefield information, greatly enhancing combat situational awareness when integrated with the existing Command, Control, and Communications, Computers, Intelligence, Surveillance and Reconnaissance (C4ISR) infrastructure. This system will provide an important boost to realizing the information dominant, network-centric objective of Joint Vision 2020. The program has established two Centers of Excellence for Sensor Technology each of which is capable of designing and building next generation, networked microsensor systems. The Defense Microelectronics Activity has teamed with the Centers of Excellence and industry to preserve long-term Department of Defense access to key next generation manufacturing technologies.

The paper presents design and performance of miniaturized chemical sensors based on silicon transducers: ion-sensitive field effect transistor (ISFET) and solid-state electrode (SSE). The sensors were fabricated as back-side contact structures, which facilitate their mounting in a flow-cell. The role of an intermediate layer between the transducer and the ion-selective membrane is discussed. Various polymeric matrices were used to manufacture microsensors: polysiloxanes, polyacrylates (polymethacrylates), polyurethanes. PMID:18969402

Depolarized Interferometric Fiber Optic Gyroscopes (D-IFOGs) that are constructed with inexpensive single mode (SM) fiber have provided an opportunity for developers to meet Army emerging missions goals for affordable, small volume, reliable inertial guidance systems for use in small missiles, munitions, and future micro-unmanned autonomous vehicles. However, there remain several vital issues associated with substantially reducing the diameter of the sensor coil. Optical fiber that is precision-wound onto a micro coil experiences increased stress due to small radius bending, fiber distortions at crossover sites, and increased interlayer pressures as a result of multiple layers of fiber wound under tension. Tension and small radius bending stresses can have a detrimental effect on the performance of D-IFOGs. Therefore, other scenarios for the application of SM fiber to a micro-sensor coil must be considered. One scheme involves taking advantage of the bending-induced birefringence and employing the low cost SM fiber as a polarization-maintaining (PM) fiber. The mechanics of how a substantial reduction in the coil radius produces PM fiber properties in SM fiber is investigated under this research effort. Conventional and specialty SM fibers are characterized to identify optimal fibers for the development of micro-sensor coils. The results from extinction ratio measurements on the SM fibers and micro-sensor coils are presented in this paper. The significant cross coupling suggests that scattering centers are present in very small radius bending. Also, measurements show that optical loss is significant in micro IFOG coils.

Dental biofilms are characterized by structural and functional heterogeneity. Due to bacterial metabolism, gradients develop and diverse ecological microniches exist. The aims of this study were (i) to determine the metabolic activity of microorganisms in naturally grown dental biofilms ex vivo by measuring dissolved oxygen (DO) and pH profiles with microelectrodes with high spatial resolution and (ii) to analyze the impact of an antimicrobial chlorhexidine (CHX) treatment on microbial physiology during stimulation by sucrose in real time. Biofilms were cultivated on standardized human enamel surfaces in vivo. DO and pH profiles were measured in a flow cell system in sterile human saliva, after sucrose addition (10%), again after alternative treatment of the sucrose exposed biofilms with CHX (0.2%) for 1 or 10 min or after being killed with paraformaldehyde (4%). Biofilm structure was visualized by vitality staining with confocal microscopy. With saliva as the sole nutrient source oxygen consumption was high within the superficial biofilm layers rendering deeper layers (>220 μm) anoxic. Sucrose addition induced the thickness of the anaerobic zone to increase with a concurrent decrease in pH (7.1 to 4.4). CHX exposure reduced metabolic activity and microbial viability at the biofilm surface and drove metabolic activity deeper into the biofilm. CHX treatment led to a reduced viability at the biofilm surface with minor influence on overall biofilm physiology after 1 min; even after 10 min there was measurable respiration and fermentation inside the biofilm. However, the local microenvironment was more aerated, less acidogenic, and presumably less pathogenic. PMID:20118374

A highly selective liquid membrane nitrite microsensor based on the hydrophobic ion-carrier aquocyanocobalt(III)-hepta(2-phenylethyl)-cobrynate is described. The sensor has a tip diameter of 10 to 15 (mu)m. The response is log-linear in freshwater down to 1 (mu)M NO(inf2)(sup-) and in seawater to 10 (mu)M NO(inf2)(sup-). A method is described for preparation of relatively large polyvinyl chloride (PVC)-gelled liquid membrane microsensors with a tip diameter of 5 to 15 (mu)m, having a hydrophilic coating on the tip. The coating and increased tip diameter resulted in more sturdy sensors, with a lower detection limit and a more stable signal than uncoated nitrite sensors with a tip diameter of 1 to 3 (mu)m. The coating protects the sensor membrane from detrimental direct contact with biomass and can be used for all PVC-gelled liquid membrane sensors meant for profiling microbial mats, biofilms, and sediments. Thanks to these improvements, liquid membrane sensors can now be used in complex environmental samples and in situ, e.g., in operating bioreactors. Examples of measurements in denitrifying, nitrifying, and nitrifying/denitrifying biofilms from wastewater treatment plants are shown. In all of these biofilms high nitrite concentrations were found in narrow zones of less than 1 mm. PMID:16535560

There is an urgent need for new chemical sensors for defense and security applications. In particular, sensors are required that can provide higher sensitivity and faster response in the field than existing baseline technologies. We have been developing a new solid-state chemical sensor technology based on microscale polymer composite fiber arrays. The fibers consist of an insulating polymer doped with conducting particles and are electrospun directly onto the surface of an interdigitated microelectrode. The concentration of the conducting particles within the fiber is controlled and is near the percolation threshold. Thus, the electrical resistance of the polymer fiber composite is very sensitive to volumetric changes produced in the polymer by vapor absorption. Preliminary results are presented on the fabrication and testing of the new microsensor. The objective is to take advantage of the very high surface to volume ratio, low thermal mass and linear geometry of the composite fibers to produce sensors exhibiting an extremely high vapor sensitivity and rapid response. The simplicity and low cost of a resistance-based chemical microsensor makes this sensing approach an attractive alternative to devices requiring RF electronics or time-of-flight analysis. Potential applications of this technology include battlespace awareness, homeland security, environmental surveillance, medical diagnostics and food process monitoring.

Nanoscale pH evaluation is a prerequisite for understanding the processes and phenomena occurring at solid-liquid, liquid-liquid, and liquid-gas interfaces, e.g., heterogeneous catalysis, extraction, partitioning, and corrosion. Research on the homogeneous processes within small volumes such as intracellular fluids, microdroplets, and microfluidic chips also requires nanometer scale pH assessment. Due to the opacity of numerous systems, optical methods are useless and, if applicable, require addition of a pH-sensitive dye. Potentiometric probes suffer from many drawbacks such as potential drift and lack of selectivity. Here, we present a voltammetric nanosensor for reliable pH assessment between pH 2 and 12 with high spatial resolution. It consists of a pyrolytic carbon nanoelectrode obtained by chemical vapor deposition (CVD) inside a quartz nanopipette. The carbon is modified by adsorption of syringaldazine from its ethanolic solution. It exhibits a stable quasi-reversible cyclic voltammogram with nearly Nernstian dependency of midpeak potentials (-54 mV/pH). This sensor was applied as a probe for scanning electrochemical microscopy (SECM) in order to map pH over a platinum ultramicroelectrode (UME), generating hydroxide ions (OH(-)) by the oxygen reduction reaction (ORR) at a diffusion-controlled rate in aerated phosphate buffered saline (PBS). The results reveal the alkalization of the electrolyte close to the oxygen reducing electrode, showing the insufficient buffer capacity of PBS to maintain a stable pH at the given conditions. PMID:26516786

We introduce a truly modular, power-aware, distributed microsensor architecture, capable of seamlessly spanning performance metrics from point-optimized low-power to point-optimized high-power applications. This type of performance is often needed in unattended ground sensor applications such as acoustic sensing and tracking, where long periods of minimal sensing activity are intermixed with short periods of intense sensor processing. The system design and implementation of a microsensor platform based on this architecture are described with experimental results. We show that although building a modular power-aware system requires additional hardware components, it results in system capable of rapid physical hardware and software reconfiguration with module reuse for new applications, while achieving a significant decrease in overall system power.

Poly-Alizarin red S/multiwalled carbon nanotube film on the surface of glassy carbon electrode (poly-AzrS/MWCNT/GCE) was synthesized by electrochemical process and was used for the sensitive and selective determination of dopamine (DA) by employing voltammetric techniques. The electrocatalytic response of the modified electrode was found to exhibit admirable activity. The simultaneous determination of dopamine in the presence of serotonin (5-HT) was found to exhibit very good response at poly-AzrS/MWCNTs/GCE. The effect of pH, scan rate, accumulation time and concentration of dopamine was studied at the developed poly-AzrS/MWCNTs/GCE. The poly-AzrS/MWCNTs/GCE exhibited an efficient electron mediating behavior together with well resolved peaks for dopamine, in 0.1mol/dm(3) phosphate buffer (PBS) solution of pH7.0. The limit of detection (LOD) and limit of quantification (LOQ) were found to be as 1.89×10(-7)mol/dm(3) and 6.312×10(-7)mol/dm(3) respectively with a dynamic range from 1×10(-6) to 1.8×10(-5)mol/dm(3). The interfacial electron transfer behavior of DA was studied by electrochemical impedance spectroscopy (EIS); the studies showed that the charge transfer rate was enhanced at poly-AzrS/MWCNTs/GCE when compared with bare GCE and poly-AzrS/GCE. PMID:26952453

Non-invasive tools that allow real-time quantification of molecules relevant to metabolism, homeostasis, and cell signaling in cells and tissue are of great importance for studying physiology. Several microsensor technologies have been developed to monitor concentration of molecules such as ions, oxygen, electroactive molecules (e.g., nitric oxide, hydrogen peroxide), and biomolecules (e.g., sugars, hormones). The major challenges for microsensors are overcoming relatively low sensitivity and low signal-to-noise ratio. Modern approaches for enhancing microsensor performance focus on the incorporation of catalytic nanomaterials to increase sensitivity, reduce response time, and increase operating range. To improve signal-to-noise ratio, a non-invasive microsensor modality called self-referencing (SR) is being applied. The SR technique allows measurement of temporal and spatial transport dynamics at the cell, tissue, organ, and organismal level.

We have developed an optical microsensor to quantify fluorescent light intensity distribution in biofilms. The optical system consisted of a beam splitter, light couplers, filters and a spectrophotometer able to accept the fiberoptic cable to measure fluorescent light intensity. The emitted light, fluorescence from the biofilm, was collected at the tip of the optical microsensor and was transferred to a spectrophotometer via a fiberoptic cable. The total fluorescent light intensity was evaluated from the emission spectrum by numerical integration. The newly developed fiberoptic microsensor was tested using a Staphylococcus aureus strain producing yellow fluorescent protein (YFP) grown as biofilm. We used a 405-nm violet laser diode for excitation, and measured the emission intensity between 480 nm and 540 nm. The optical microsensor that quantifies fluorescent light intensity is a promising tool in biofilm research which often requires detection and quantification of fluorescent light intensity distribution generated by various fluorescent proteins. PMID:15279941

An interface circuit in a 0.8-micrometers CMOS process for the on- chip integration of a capacitive micro-sensor used as a microphone is presented. In order to circumvent 1/f noise contributions and to improve the signal/noise ratio, a synchronous modulation-demodulation technique has been applied. For the implementation of this technique, we have studied and designed several functional block, such as modulator with signal conversion, low-noise amplifier, demodulator, etc. To deal with problems related to dispersion of intrinsic capacitance of the sensor, a feedback compensating solution is suggested. The designed circuit has a sensibility of 1200 V/pF, with a minimum detectable capacitance variation of 2 10-6 pF.

Microscale fiber tip sensors based on the plasmon resonance are reported. The fabrication process derived from our previous approach for manufacturing near-field scanning optical microscopy probes has been optimized for sensing applications. A typical tip sensor is a tapered fiber 400 microm in length, coated with a nanoporous thin silver film. The miniaturized geometry of the sensor allows detection in a single droplet of liquid solution (approximately 20 microl). The tip sensor is sensitive for refractive indices between 1.33 and 1.40 with a sensitivity of at least 3 x 10(-4) refractive index unit (RIU)/nm. The Raman scattering enhancement through these microsensors demonstrates the important role played by the localized plasmon resonance. The sensors' linear response covers a large region, interesting for biosensing in aqueous environments such as biomedical applications. PMID:17700810

Recent advances in technology involving magnetic materials require development of novel advanced magnetic materials with improved magnetic and magneto-transport properties and with reduced dimensionality. Therefore magnetic materials with outstanding magnetic characteristics and reduced dimensionality have recently gained much attention. Among these magnetic materials a family of thin wires with reduced geometrical dimensions (of order of 1–30 μm in diameter) have gained importance within the last few years. These thin wires combine excellent soft magnetic properties (with coercivities up to 4 A/m) with attractive magneto-transport properties (Giant Magneto-impedance effect, GMI, Giant Magneto-resistance effect, GMR) and an unusual re-magnetization process in positive magnetostriction compositions exhibiting quite fast domain wall propagation. In this paper we overview the magnetic and magneto-transport properties of these microwires that make them suitable for microsensor applications. PMID:22291562

An amperometric solid electrolyte oxygen (O2) microsensor using a novel and robust structure has been developed with a detection range of 0.025 to 21 percent of O2 concentration. The microsensor has a simple structure with a sensing area of 1.10 0.99 mm(exp 2), and is operated by applying voltage across the electrodes and measuring the resulting current flow at a temperature of 600 C.

Capacitive sensing schemes are widely used for various microsensors; however, such microsensors suffer from severe parasitic capacitance problems. This paper presents a fully integrated low-noise readout circuit with automatic offset cancellation loop (AOCL) for capacitive microsensors. The output offsets of the capacitive sensing chain due to the parasitic capacitances and process variations are automatically removed using AOCL. The AOCL generates electrically equivalent offset capacitance and enables charge-domain fine calibration using a 10-bit R-2R digital-to-analog converter, charge-transfer switches, and a charge-storing capacitor. The AOCL cancels the unwanted offset by binary-search algorithm based on 10-bit successive approximation register (SAR) logic. The chip is implemented using 0.18 μm complementary metal-oxide-semiconductor (CMOS) process with an active area of 1.76 mm2. The power consumption is 220 μW with 3.3 V supply. The input parasitic capacitances within the range of −250 fF to 250 fF can be cancelled out automatically, and the required calibration time is lower than 10 ms. PMID:26473877

Capacitive sensing schemes are widely used for various microsensors; however, such microsensors suffer from severe parasitic capacitance problems. This paper presents a fully integrated low-noise readout circuit with automatic offset cancellation loop (AOCL) for capacitive microsensors. The output offsets of the capacitive sensing chain due to the parasitic capacitances and process variations are automatically removed using AOCL. The AOCL generates electrically equivalent offset capacitance and enables charge-domain fine calibration using a 10-bit R-2R digital-to-analog converter, charge-transfer switches, and a charge-storing capacitor. The AOCL cancels the unwanted offset by binary-search algorithm based on 10-bit successive approximation register (SAR) logic. The chip is implemented using 0.18 μm complementary metal-oxide-semiconductor (CMOS) process with an active area of 1.76 mm². The power consumption is 220 μW with 3.3 V supply. The input parasitic capacitances within the range of -250 fF to 250 fF can be cancelled out automatically, and the required calibration time is lower than 10 ms. PMID:26473877

Chemical microsensors rely on partitioning of airborne chemicals into films to collect and measure trace quantities of hazardous vapors. Polymer sensor coatings used today are typically slow to respond and difficult to apply reproducibly. The objective of this project was to produce a durable sensor coating material based on graphitic nanoporous-carbon (NPC), a new material first studied at Sandia, for collection and detection of volatile organic compounds (VOC), toxic industrial chemicals (TIC), chemical warfare agents (CWA) and nuclear processing precursors (NPP). Preliminary studies using NPC films on exploratory surface-acoustic-wave (SAW) devices and as a {micro}ChemLab membrane preconcentrator suggested that NPC may outperform existing, irreproducible coatings for SAW sensor and {micro}ChemLab preconcentrator applications. Success of this project will provide a strategic advantage to the development of a robust, manufacturable, highly-sensitive chemical microsensor for public health, industrial, and national security needs. We use pulsed-laser deposition to grow NPC films at room-temperature with negligible residual stress, and hence, can be deposited onto nearly any substrate material to any thickness. Controlled deposition yields reproducible NPC density, morphology, and porosity, without any discernable variation in surface chemistry. NPC coatings > 20 {micro}m thick with density < 5% that of graphite have been demonstrated. NPC can be 'doped' with nearly any metal during growth to provide further enhancements in analyte detection and selectivity. Optimized NPC-coated SAW devices were compared directly to commonly-used polymer coated SAWs for sensitivity to a variety of VOC, TIC, CWA and NPP. In every analyte, NPC outperforms each polymer coating by multiple orders-of-magnitude in detection sensitivity, with improvements ranging from 103 to 108 times greater detection sensitivity! NPC-coated SAW sensors appear capable of detecting most analytes tested to

Microrobots are the result of increasing research activities at the border between microsystem technology and robotics. Today already, robots with dimensions of a few cubic- centimeters can be developed. Like conventional robots, microrobots represent a complex system that usually contains several different types of actuators and sensors. The measurement of gripping forces is the most important sensor application in micromanipulation besides visual servoing to protect the parts from too high surface pressures and thereby damage during the assembly process. Very small forces in the range of 200 (mu) N down to 0.1 (mu) N or even less have to be sensed. Thus, the aim of our current research activities is the development of a high-resolution integrated force microsensor for measuring gripping forces in a microhandling robot. On the one hand, the sensor should be a device for teleoperated manipulation tasks in a flexible microhandling station. On the other hand, typical microhandling operations should to a large extend be automated with the aid of computer-based signal processing of sensor information. The user should be provided with an interface for teleoperated manipulation and an interface for partially automated manipulation of microobjects. In this paper, a concept for the measurement of gripping forces in microrobotics using piezoresistive AFM (atomic force microscope) cantilevers is introduced. Further on, the concept of a microrobot-based SEM station and its applications are presented.

Important factors in the application of sensing technology to space applications are low mass, small size, and low power. All of these attributes are enabled by the application of MEMS and micro-fabrication technology to microsensors. Two types of sensors are utilized in space applications: remotes sensing from orbit around the earth or another planetary body, and point sensing in the spacecraft or external to it. Several Sandia projects that apply microfabrication technologies to the development of new sensing capabilities having the potential for space applications will be briefly described. The Micro-Navigator is a project to develop a MEMS-based device to measure acceleration and rotation in all three axes for local area navigation. The Polychromator project is a joint project with Honeywell and MIT to develop an electrically programmable diffraction grating that can be programmed to synthesize the spectra of molecules. This grating will be used as the reference cell in a gas correlation radiometer to enable remote chemical detection of most chemical species. Another area of research where microfabrication is having a large impact is the development of a lab on a chip. Sandia's efforts to develop the {mu}ChemLab{trademark} will be described including the development of microfabricated pre-concentrators, chromatographic columns, and detectors. Smart sensors that allow the spacecraft independent decision making capabilities depend on pattern recognition. Sandia's development of a new pattern recognition methodology that can be used to interpret sensor response as well as for target recognition applications will be described.

Solid-state microelectrodes have been used in situ in Raritan Bay, NJ to measure pore water profiles of dissolved O{sub 2}, Mn, Fe, and sulfide at (sub)millimeter resolution by voltammetric techniques. The voltammetric sensor was positioned with microprofiling instrumentation mounted on a small remote operated vehicle (ROV). This instrumentation and the sensor were controlled and monitored in real time from a research vessel anchored at the study site. The voltammetric analyzer was connected to the electrodes of the voltammetric cell with a 30 m cable which also bridged receiver-transmitter transducers to ensure signal quality along the cable. Single analyte O{sub 2}, pH, and resistivity microsensors were operated alongside the voltammetric sensor. The authors report on the technology of the system and the concentration changes of redox species observed from 2 to 3 cm above to approximately 4 cm below the sediment-water interface during three deployments. O{sub 2} measurements from both Clark and voltammetric electrodes were in excellent agreement. The profiles obtained show that there is no detectable overlap of O{sub 2} and Mn{sup 2+} in the sediments which is similar to previous reports from other continental margin sediments which were cored and analyzed in the laboratory. These data indicate that O{sub 2} is not a direct oxidant for Mn{sup 2+} when diffusive (rather than advective) processes control the transport of solutes within the sediment. Subsurface Mn{sup 2+} peaks were observed at about 2 cm and coincide with a subsurface pH maximum. The data can be explained by organic matter decomposition with alternate electron acceptors and by the formation of authigenic phases containing reduced Mn at depth.

We report the fabrication and electrochemical response of a gold nanoband electrode located at the bottom of a glass/epoxy nanotrench, hereafter referred to as a gold nanotrench electrode. Gold nanotrench electrodes of 12.5 and 40 nm in width with various depths from a few tens of nanometers to approximately 4 μm are fabricated and further characterized by cyclic voltammetry. The fabrication of a Au nanotrench electrode follows a simple electrochemical etching process in which a small AC signal is applied to an inlaid Au nanoband electrode submersed in a NaCl solution. The voltammetric behavior of a Au nanotrench electrode is characterized by a quasi-steady-state response at lower scan rates (e.g., <1 V/s for a 12.5-nm-wide electrode). We present an analytical expression for the quasi-steady-state diffusion-limited current of the nanotrench electrode based upon the analysis of the mass-transport resistance. Finite-element simulation of steady-state and transient voltammetric responses of the nanotrench electrodes provides additional insights for the analytical model. Peak-shaped transient voltammetric responses were observed at scan rates as low as 5 V/s for both inlaid and nanotrench electrodes. This result may suggest that the exposed area of the nanoband electrode is much greater than that expected from the fabrication of the inlaid bands. However, the extent to which this is seen is greatly decreased in the nanotrench electrode by a smoothing effect during etching. Our results confirm previous reports of excess overhanging metal and delamination crack contributing significantly to the shape and magnitude of the voltammetric response. PMID:21866978

Two new compounds (8-H 2Q) 2[M(dipic) 2]·6H 2O (M = Co ( 1) and Ni ( 2), 8-HQ = 8-hydroxyquinoline, dipic = dipicolinate) have been prepared and characterized by elemental analysis, spectral (IR and UV-vis), thermal analyses, magnetic measurements and single-crystal X-ray diffraction techniques. Both 1 and 2 consist two 8-hydroxyquinolinium cations, one bis(dipicolinate)M(II) anion [M = Co(II), Ni(II)] and six uncoordinated water molecules. Both 1 and 2 crystallize in the monoclinic space group C2/c. In the compounds anion, each dipic ligand simultaneously exhibits tridentate coordination modes through N atom of pyridine ring and oxygen atoms of the carboxylate groups. The crystal packing of 1 and 2 is a composite of intermolecular hydrogen bonding and C-O&ctdot;π interactions. The in vitro antibacterial and antifungal activities of 1 and 2 were evaluated by the agar well diffusion method by MIC tests. Both new compounds showed the same antimicrobial activity against Gram-positive bacteria and yeast and fungi expect Gram-negative bacteria.

A highly selective needle type solid state amperometric nitrite microsensor based on direct nitrite oxidation on carbon fiber was developed using a simplified fabrication method. The microsensor’s tip diameter was approximately 7 µm, providing a high spatial resolution of at lea...

MEMS are currently being applied to the structural health monitoring of critical aircraft components and composites. The approach integrates acoustic emission, strain gauges, MEMS accelerometers and vibration monitoring aircraft components with a known history of catastrophic failure due to fracture. Recently a combination of the need for safety in the air and the desire to control costs is encouraging the use of in-flight monitoring of aircraft components and systems using light-weight, wireless and cost effective microsensors and MEMS. An in-situ aircraft structural health monitoring system, with sensors embedded in the composite structure or surface-mounted on the structure, would permit the timely detection of damage in aircraft. Micromachining offers the potential for fabricating a range of microsensor and MEMS for structural applications including load, vibration and acoustics characterization and monitoring. Such microsensors are extremely small; they can be embedded into structural materials, can be mass-produced and are therefore potentially cheap. The smart sensors are being developed using the standard microelectronics and micromachining in conjunction with novel Penn State wireless communication systems suitable for condition monitoring of aircraft structures in-flight. The main application areas of this investigation include continuos monitoring of a) structural integrity of aging aircraft, b) fatigue cracking, c) corrosion, d) deflection and strain of aircraft structures, wings, and rotorblades, e) impact damage, f) delamination and g) location and propagation of cracks. In this paper we give an overview of wireless programmable microsensors and MEMS and their associated driving electronics for such applications.

Plant experiments in space will require active nutrient delivery concepts in which water and nutrients are replenished on a continuous basis for long-term growth. The goal of this study is to develop a novel microsensor array to provide information on the dissolved oxygen environment in the plant root zone for the optimum control of plant cultivation systems in the space environment. Control of water and oxygen is limited by the current state-of-the-art in sensor technology. Two capabilities of the new microsensor array were tested. First, a novel in situ self-diagnosis/self-calibration capability for the microsensor was explored by dynamically controlling the oxygen microenvironment in close proximity to an amperometric dissolved oxygen microsensors. A pair of integrated electrochemical actuator electrodes provided the microenvironments based on water electrolysis. Miniaturized thin film dissolved oxygen microsensors on a flexible polyimide (Kapton(Registered Trademark)? substrate were fabricated and their performances were tested. Secondly, measurements of dissolved oxygen in two representative plant growth systems were made, which had not been performed previously due to lack of proper sensing technology. The responses of the oxygen microsensor array on a flexible polymer substrate properly reflected the oxygen contents on the surface of a porous tube nutrient delivery system and within a particulate substrate system. Additionally, we demonstrated the feasibility of using a 4-point thin film microprobe for water contents measurements for both plant growth systems. mechanical flexibility, and self-diagnosis. The proposed technology is anticipated to provide a reliable sensor feedback plant growth nutrient delivery systems in both terrestrial environment and the microgravity environment during long term space missions. The unique features of the sensor include small size and volume, multiple-point sensing,

Electro-active polymers are emerging in the fields of actuators and micro-sensors because their good dielectric and mechanical properties makes them suitable for such applications. In this work, we focus on micro-structured (cellular) polymer materials (referred as piezoelectrets or ferroelectrets) that need prior charging to attain piezoelectric behaviour. The development of such applications requires an in-depth knowledge of the intrinsic dielectric properties of such structures and models to enable the accurate prediction of a given micro-structured material’s dielectric properties. Various polymers including polypropylene, polytetrafluoroethylene, fluoroethylenepropylene, cyclo-olefines and poly(ethylene terephthalate) in a cellular form have been studied by researchers over the last fifteen years. However, there is still a lack of information on the intrinsic dielectric properties of the most recently used dielectric polymer (polydimethylsiloxane, PDMS) over wide frequency and temperature ranges. In this work, we shall propose an exhaustive equivalent electrical circuit model and explain how it can be used to predict the micro-structured PDMS complex permittivity versus frequency and temperature. The results obtained from the model were found to be in good agreement with experimental data for various micro-structured PDMS materials. Typically, for micro-sensor applications, the dielectric constant and dielectric losses are key factors which need to be minimized. We have developed a configuration which enables both to be strongly reduced with a reduction of 16% in the dielectric constant of a micro-structured PDMS compared with the bulk material. In addition, the phenomena responsible for dielectric losses variations with frequency and temperature are discussed and correlated with the theoretical model. Our model is thus proved to be a powerful tool for the control of the dielectric properties of micro-structured PDMS material for micro-sensor applications.

Poly(carbon disulfide) was studied by cyclic voltammetry using glassy carbon and platinum macro- and microdisk electrodes. The electron transfer kinetics is significantly faster at glassy carbon electrodes than at Pt electrodes. It is chemically reversible with moderate electron transfer rates. Voltammetric results of poly(carbon disulfide) are in good agreement with battery testing data. The k{sup 0} value measured at a Pt microdisk electrode is 7{times}10{sup 3} cm/sec. Electrochemical data suggest that PCS can be a potential cathode material for low current density lithium batteries.

A novel gas-sensitive microsensor, whose design is based upon the interdigitated-gate-electrode field-effect transistor was realized by integrating it with ia selectively-deposited, chemically-active, electron-beam evaporated copper phthalocyanine (CuPc) thin film. When isothermally operated at 150 degrees C, the microsensor can selectively and reversibly detect parts-per-billion (ppb) concentration levels of two environmentally-sensitive pollutants, nitrogen dioxide (NO2) and diisopropyl methylphosphonate (DIMP). Although the CuPc thin film chemically and electrically interacts with NO2 and DIMP, just as it will likely interact with other electrically- active gases, or combinations thereof, the selectivity feature of the microsensor was established by operating it with a 5-V peak amplitude, 2-microsecond(s) duration, 1000 Hz repetition frequency pulse, and then analyzing its time- and frequency-domain responses. As a direct consequence of this analysis, the envelopes associated with the normalized- difference Fourier transform magnitude frequency spectra reveal features which unambiguously distinguish the NO2 and DIMP challenge gas responses. Furthermore, the area beneath each response envelope may correspondingly be interpreted as a metric for the microsensor's sensitivity to a specific challenge gas concentration. Scanning electron microscopy was used to characterize the CuPc thin film's morphology. Additionally, infrared spectroscopy was employed to verify the (alpha) - and (beta) -phases of the sublimed CuPc thin films and to study the NO2- and DIMP-CuPc interactions.

A multitude of industries use H2 either as part of their process or as a fuel. All these applications motivate nowadays the development of hydrogen sensor devices which enable its safe and controlled use. Since H2 is explosive above the lower explosion limit at 40,000 ppm, devices which permit the detection of its presence and measure its concentration become indispensable. In this work, we present a microsensor based on NiO thin films produced with dc reactive magnetron sputtering on GaAs, with an incorporated Pt heater, all on a DO-8 package ready for use. The microsensor was tested to H2 concentrations 5,000 and 10,000 ppm at different working temperatures. The change of the electrical resistance of NiO thin films was the signal for hydrogen sensing. The response of the sensor was not proportional to concentration of the gas neither to the working temperature.

An article of manufacture is provided including a substrate having an oxide surface layer and a layer of a cyclodextrin derivative chemically bonded to said substrate, said layer of a cyclodextrin derivative adapted for the inclusion of selected compounds, e.g., nitro-containing organic compounds, therewith. Such an article can be a chemical microsensor capable of detecting a resultant mass change from inclusion of the nitro-containing organic compound.

We report on the fabrication of photo-driven polymer microsensors for viscosimetry, velocimetry and micropump applications. They are readily made with a low-cost polymerization technique based on two-photon absorption. Microsensors are free-floating in the liquid to be characterized. A linearly-polarized optical tweezers is used to trap one sensor at the laser focal point and to generate the optical torque needed for local hydrodynamic measurements. Viscosity and velocity microsensors have slab shapes that align in the polarization direction. The local viscosity is deduced from the maximum rotation frequency generated by the rotating linear polarization, while the fluid velocity is obtained by measuring the maximum angle that equilibrates the optical torque and drag torque. Experimental results are in good agreement with theoretical calculations. The micropump is based on a micron-size Archimedes screw that rotates around its long axis when it is trapped at the focal point. The laser-induced rotation is due to the optical torque that is transferred by the laser scattering on the screw.

High sensitivity acoustic wave chemical microsensors are being developed on GaAs substrates. These devices take advantage of the piezoelectric properties of GaAs as well as its mature microelectronics fabrication technology and nascent micromachining technology. The design, fabrication, and response of GaAs SAW chemical microsensors are reported. Functional integrated GaAs SAW oscillators, suitable for chemical sensing, have been produced. The integrated oscillator requires 20 mA at 3 VK, operates at frequencies up to 500 MHz, and occupies approximately 2 mmz. Discrete GaAs sensor components, including IC amplifiers, SAW delay lines, and IC phase comparators have been fabricated and tested. A temperature compensation scheme has been developed that overcomes the large temperature dependence of GaAs acoustic wave devices. Packaging issues related to bonding miniature flow channels directly to the GaAs substrates have been resolved. Micromachining techniques for fabricating FPW and TSM microsensors on thin GaAs membranes are presented and GaAs FPW delay line performance is described. These devices have potentially higher sensitivity than existing GaAs and quartz SAW sensors.

Monolithic, integrated acoustic wave chemical microsensors are being developed on gallium arsenide (GaAs) substrates. With this approach, arrays of microsensors and the high frequency electronic components needed to operate them reside on a single substrate, increasing the range of detectable analytes, reducing overall system size, minimizing systematic errors, and simplifying assembly and packaging. GaAs is employed because it is both piezoelectric, a property required to produce the acoustic wave devices, and a semiconductor with a mature microelectronics fabrication technology. Many aspects of integrated GaAs chemical sensors have been investigated, including: surface acoustic wave (SAW) sensors; monolithic SAW delay line oscillators; GaAs application specific integrated circuits (ASIC) for sensor operation; a hybrid sensor array utilizing these ASICS; and the fully monolithic, integrated SAW array. Details of the design, fabrication, and performance of these devices are discussed. In addition, the ability to produce heteroepitaxial layers of GaAs and aluminum gallium arsenide (AlGaAs) makes possible micromachined membrane sensors with improved sensitivity compared to conventional SAW sensors. Micromachining techniques for fabricating flexural plate wave (FPW) and thickness shear mode (TSM) microsensors on thin GaAs membranes are presented and GaAs FPW delay line and TSM resonator performance is described.

Development of a taste sensor with high sensitivity, stability and selectivity is highly desirable for the food and beverage industries. The main goal of a taste sensor is to reproduce five kinds of senses of humans, which is quite difficult. The importance of knowing quality of beverages and drinking water has been recognized as a result of increase in concern in environmental pollution issues. However, no accurate measuring system appropriate for quality evaluation of beverages is available. A highly sensitive microsensor using horizontally polarized Surface Acoustic Waves (SH-SAW) for the detection and identification of soft drinks is presented in this paper. Different soft drinks were tested using this sensor and the results which could distinguish between two popular soft drinks like Pepsi and Coca cola is presented in this paper. The SH-SAW microsensors are fabricated on 36°-rotated Y cut X propagating LiTaO3 (36YX.LT) substrate. This design consists of a dual delay line configuration in which one line is free and other one is metallized and shielded. Due to high electromechanical coupling of 36YX.LT, it could detect difference in electrical properties and hence to distinguish different soft drinks. Measured electrical characteristics of these soft drinks at X-band frequency using free space system show distinguishable results. It is clear from these results that the microsensor based on 36YX.LT is an effective liquid identification system for quantifying human sensory expressions.

Polyphenolic compounds are electrochemically active components of vegetal matter which were targeted under simple experimental conditions to produce voltammetric profiles characterizing the metabolite composition. Application to bivariate and multivariate chemometric techniques permits to discriminate the species and age of plant leaves, illustrated here for the case of six Pinus species from two different subgenera. Such responses, associated with the electrochemical oxidation of polyphenolic compounds (quercetin, gallic acid, ellagic acid, among others), define a voltammetric profile which varies systematically with the age of the leaves for the different species. The application of this methodology for phylogenetic studies, plant physiology, forensic science, and chemoecology is discussed. Graphical Abstract Image of Pinus in a typical Mediterranean forest; Courtesy of the Botanic Garden of the University of Valencia. PMID:27173392

The integration of MEMS, IDTs (interdigital transducers) and required microelectronics and conformal antennas to realize programmable, robust and low cost passive microsensors suitable for many military structures and systems including aircraft, missiles and munitions is presented in this paper. The technology is currently being applied to the structural health monitoring of critical aircraft components. The approach integrates acoustic emission, strain gauges, MEMS accelerometers, gyroscopes and vibration monitoring devices with signal processing electronics to provide real-time indicators of incipient failure of aircraft components with a known history of catastrophic failure due to fracture. Recently a combination of the need for safety in the air and the desire to control costs is encouraging the use of in-flight monitoring of aircraft components and systems using light-weight, wireless and cost effective microsensors and MEMS. An in-situ Aircraft structural health monitoring (ASHM) system, with sensors embedded in the composite structure or surface-mounted on the structure, would permit the timely detection of damage in aircraft. Micromachining offers the potential for fabricating a range of microsensors and MEMS for structural applications including load, vibration and acoustics characterization and monitoring. Such microsensors are extremely small; they can be embedded into structural materials, can be mass-produced and are therefore potentially cheap. Additionally a range of sensor types can be integrated onto a single chip with built-in electronics and ASIC (Application Specific Integrated Circuit), providing a low power Microsystems. The smart sensors are being developed using the standard microelectronics and micromachining in conjunction with novel Penn State smart electronics or wireless communication systems suitable for condition monitoring of aircraft structures in-flight. A hybrid accelerometer and gyroscope in a single chip suitable for inertial

The design and development of wireless mocrosensor network systems for the treatment of many degenerative as well as traumatic neurological disorders is presented in this paper. Due to the advances in micro and nano sensors and wireless systems, the biomedical sensors have the potential to revolutionize many areas in healthcare systems. The integration of nanodevices with neurons that are in communication with smart microsensor systems has great potential in the treatment of many neurodegenerative brain disorders. It is well established that patients suffering from either Parkinson"s disease (PD) or Epilepsy have benefited from the advantages of implantable devices in the neural pathways of the brain to alter the undesired signals thus restoring proper function. In addition, implantable devices have successfully blocked pain signals and controlled various pelvic muscles in patients with urinary and fecal incontinence. Even though the existing technology has made a tremendous impact on controlling the deleterious effects of disease, it is still in its infancy. This paper presents solutions of many problems of today's implantable and neural-electronic interface devices by combining nanowires and microelectronics with BioMEMS and applying them at cellular level for the development of a total wireless feedback control system. The only device that will actually be implanted in this research is the electrodes. All necessary controllers will be housed in accessories that are outside the body that communicate with the implanted electrodes through tiny inductively-coupled antennas. A Parkinson disease patient can just wear a hat-system close to the implantable neural probe so that the patient is free to move around, while the sensors continually monitor, record, transmit all vital information to health care specialist. In the event of a problem, the system provides an early warning to the patient while they are still mobile thus providing them the opportunity to react and

We used a novel amperometric microsensor for measuring hydrogen gas production and consumption at high spatio-temporal resolution in cyanobacterial biofilms and mats dominated by non-heterocystous filamentous cyanobacteria (Microcoleus chtonoplastes and Oscillatoria sp.). The new microsensor is based on the use of an organic electrolyte and a stable internal reference system and can be equipped with a chemical sulfide trap in the measuring tip; it exhibits very stable and sulfide-insensitive measuring signals and a high sensitivity (1.5–5 pA per μmol L-1 H2). Hydrogen gas measurements were done in combination with microsensor measurements of scalar irradiance, O2, pH, and H2S and showed a pronounced H2 accumulation (of up to 8–10% H2 saturation) within the upper mm of cyanobacterial mats after onset of darkness and O2 depletion. The peak concentration of H2 increased with the irradiance level prior to darkening. After an initial build-up over the first 1–2 h in darkness, H2 was depleted over several hours due to eﬄux to the overlaying water, and due to biogeochemical processes in the uppermost oxic layers and the anoxic layers of the mats. Depletion could be prevented by addition of molybdate pointing to sulfate reduction as a major sink for H2. Immediately after onset of illumination, a short burst of presumably photo-produced H2 due to direct biophotolysis was observed in the illuminated but anoxic mat layers. As soon as O2 from photosynthesis started to accumulate, the H2 was consumed rapidly and production ceased. Our data give detailed insights into the microscale distribution and dynamics of H2 in cyanobacterial biofilms and mats, and further support that cyanobacterial H2 production can play a significant role in fueling anaerobic processes like e.g., sulfate reduction or anoxygenic photosynthesis in microbial mats. PMID:26257714

We show the technical feasibility of coating and micro patterning boron-doped ultrananocrystalline diamond (UNCD®) on metal microwires and of applying them as microsensors for the detection of dopamine in vivo using fast-scan cyclic voltammetry. UNCD electrode surface consistently generated electrochemical signals with high signal-to-noise ratio of >800 using potassium ferrocyanide-ferricyanide redox couple. Parylene patterned UNCD microelectrodes were effectively applied to detect dopamine reliably in vitro using flow injection analysis with a detection limit of 27 nM and in the striatum of the anesthetized rat during electrical stimulation of dopamine neurons. PMID:23918991

We show the technical feasibility of coating and micro patterning boron-doped ultrananocrystalline diamond (UNCD(®)) on metal microwires and of applying them as microsensors for the detection of dopamine in vivo using fast-scan cyclic voltammetry. UNCD electrode surface consistently generated electrochemical signals with high signal-to-noise ratio of >800 using potassium ferrocyanide-ferricyanide redox couple. Parylene patterned UNCD microelectrodes were effectively applied to detect dopamine reliably in vitro using flow injection analysis with a detection limit of 27 nM and in the striatum of the anesthetized rat during electrical stimulation of dopamine neurons. PMID:23918991

This study investigates the design and fabrication of magnetic microsensors using the commercial 0.35 μm complementary metal oxide semiconductor (CMOS) process. The magnetic sensor is composed of springs and interdigitated electrodes, and it is actuated by the Lorentz force. The finite element method (FEM) software CoventorWare is adopted to simulate the displacement and capacitance of the magnetic sensor. A post-CMOS process is utilized to release the suspended structure. The post-process uses an anisotropic dry etching to etch the silicon dioxide layer and an isotropic dry etching to remove the silicon substrate. When a magnetic field is applied to the magnetic sensor, it generates a change in capacitance. A sensing circuit is employed to convert the capacitance variation of the sensor into the output voltage. The experimental results show that the output voltage of the magnetic microsensor varies from 0.05 to 1.94 V in the magnetic field range of 5–200 mT. PMID:24172287

Resonant pressure microsensors are widely used in the fields of aerospace exploration and atmospheric pressure monitoring due to their advantages of quasi-digital output and long-term stability, which, however, requires the use of additional temperature sensors for temperature compensation. This paper presents a resonant pressure microsensor capable of self-temperature compensation without the need for additional temperature sensors. Two doubly-clamped “H” type resonant beams were arranged on the pressure diaphragm, which functions as a differential output in response to pressure changes. Based on calibration of a group of intrinsic resonant frequencies at different pressure and temperature values, the functions with inputs of two resonant frequencies and outputs of temperature and pressure under measurement were obtained and thus the disturbance of temperature variations on resonant frequency shifts was properly addressed. Before compensation, the maximal errors of the measured pressure values were over 1.5% while after compensation, the errors were less than 0.01% of the full pressure scale (temperature range of −40 °C to 70 °C and pressure range of 50 kPa to 110 kPa). PMID:25938197

Accurate assessments of reliability and condition based maintenance can only be implemented where a good understanding of ammunition stockpile condition exists. Use of miniaturized intelligent sensors provides an inexpensive means of nondestructively gaining insight into stockpile condition while keeping costs low. In the past, evaluation of ammunition lifetimes has utilized humidity, temperature, pressure, shock, and corrosion. New technologies provide the possibility of obtaining these environmental parameters, as well as a number of other indicators of propellant degradation, including NOx by utilizing a microsensor with capability for remote wireless monitoring. Micro-electro-mechanical systems (MEMS) like microcantilevers promise to revolutionize the field of sensor design. In the automobile industry, micromachined acceleration sensors are now used for triggering airbags and pressure sensors adjust the air-fuel intake ratio in the engine. By applying coatings to the sensor`s surface the behavior of the microdevice can be measurably altered to respond to chemical species as demonstrated by ORNL using microcantilevers to detect mercury vapor and humidity. Ultimately, single-chip detectors with electronics and telemetry could be developed with conceivably hundreds of individual microsensors on each chip to simultaneously monitor identify, and quantify many important chemical species for ammunition as well as measure environmental parameters.

Electrochemical microsensors have been applied in the field of biomedicine for many years. The aim of this work was to develop a novel oxygen sensor to monitor the partial pressure of oxygen in tissues and acupuncture points. The functions of microsensor were evaluated through in vitro experiments. In vivo in tissues and acupuncture points. The data from oxygen microsensor were compared with the data from blood gas analyzer. The measurements depend on the physiological changes of experimental animal. The further development of this new sensor is to be a tool for meridian research.

We propose a bihydrogel mechanical microsensor made from two hydrogels with different sensitivity to the environment. The idea was used to create pH microsensors consisting of two parallel phases of crosslinked hydrogel in which only one phase is pH-sensitive. Working similarly to a bimetallic strip, the bihydrogel particle bends depending on the environmental pH. These freestanding bihydrogel particles are low-cost and easy to manufacture. They are particularly suitable for use in confined environment where most microsensors are unable to fit in. The same principle can also be used to create sensors for temperature, ionic strength, and other environmental parameters.

Miniature unmanned aerial vehicles (UAVs) are a category of aircraft small enough to be transported, launched, operated, and retrieved by a crew of one or two. The concept is not new, having been in limited use by the U.S. military over the past fifteen years, but interest in potential applications is growing as size and cost of the vehicles come down. An application that is particularly significant to the military and law-enforcement agencies is remote reconnaissance, with one or more onboard sensors transmitting data back to the operator(s) in real time. Typically, a miniature UAV is capable of flying a pre-programmed route autonomously, with manual override as an option. At the conclusion of the mission, the vehicle returns for landing, after which it can be quickly disassembled and stowed until its next use. Thermal imaging extends the utility of miniature UAVs to operations in complete darkness and limited visibility, but historically thermal imagers have been too large and heavy for this application. That changed in 1999 with the introduction of Indigo System's AlphaTM camera, which established a new class of thermal imaging product termed the infrared "microsensor". Substantially smaller and lighter than any other infrared imaging product available at the time, AlphaTMwas the first camera that could be readily packaged into the nose of a miniature UAV. Its low power consumption was also a key enabling feature. Building upon the success of AlphaTM, Indigo then took the microsensor class a step further with its OmegaTM camera, which broke all the records established by AlphaTM for small size, weight, and power. OmegaTM has been successfully integrated into several miniature UAVs, including AeroVironment's Pointer and Raven, as well as the Snake Eye UAV manufactured by BAI Aerosystems. Aspects of the OmegaTM design that have led to its utility on these and other platforms are described, and future prospects for even smaller microsensors are discussed.

Chemical sensors are used in a wide variety of applications, such as environmental monitoring, fire detection, emission monitoring, and health monitoring. The fabrication of chemical sensors involving nanostructured materials holds the potential for the development of sensor systems with unique properties and improved performance. However, the fabrication and processing of nanostructures for sensor applications currently are limited in the ability to control their location on the sensor, which in turn hinders the progress for batch fabrication. This report discusses the advantages of using nanomaterials in sensor designs, some of the challenges encountered with the integration of nanostructures into microsensor / devices, and then briefly describes different methods attempted by other groups to address this issue. Finally, this report will describe how our approach for the controlled alignment of nanostructures onto a sensor platform was applied to demonstrate an approach for the mass production of sensors with nanostructures.

Scientists at Argonne (IL) National Laboratory have developed a thin-film microsensor that is capable of detecting and quantifying a wide variety of gases and gas mixtures at concentraitons as low as 1 ppm. The sensor technology is suitable for controlling boiler and flue-gas emissions, characterizing contaminated soil and air, monitoring for noxious gases, and providing early intelligent detection of toxic vapors. Intelligence comes from onboard neural network software that identifies gases by matching cyclic voltammograms with stored patterns previously obtained from standard reference samples. The sensor and the techniques used to optimize the thin films involved will be the subject of a talk given by Jim Vetrone on Tuesday aternoon at 2:20 p.m. in Room 1011.

Commercialization of a competitive reusable launch vehicle (RLV) is a primary goal for both NASA and the U.S. aerospace industry. To expedite achievement of this goal, the Bantam-X Technology Program is funding development of innovative technologies to lower costs for access to space. Ground operations is one area where significant cost reduction is required. For the Shuttle fleet, ground operations account for over 80% of the life cycle costs, and TPS recertification accounts for 27% of the operation costs ($4.5M per flight). Bantam Task TPS-7, Subsurface Microsensors for Assisted Recertification of TPS (SmarTPS), is a joint effort between NASA centers and industry partners to develop rapid remote detection and scanning technology for inspection of TPS and detection of subsurface defects. This short paper will provide a general overview of the SmarTPS concept.

A simple method based on the multivariate analysis of data from urine using an electronic voltammetric tongue is used to detect patients with prostate cancer. A sensitivity of 91% and a specificity of 73% were obtained to distinguish the urine from cancer patients and the urine from non-cancer patients. PMID:27375181

A sensitive resistor-based NO microsensor, with a wide detection range and a low detection limit, has been developed. Semiconductor microfabrication techniques were used to create a sensor that has a simple, robust structure with a sensing area of 1.10 0.99 mm. A Pt interdigitated structure was used for the electrodes to maximize the sensor signal output. N-type semiconductor indium tin oxide (ITO) thin film was sputter-deposited as a sensing material on the electrode surface, and between the electrode fingers. Alumina substrate (250 m in thickness) was sequentially used for sensor fabrication. The resulting sensor was tested by applying a voltage across the two electrodes and measuring the resulting current. The sensor was tested at different concentrations of NO-containing gas at a range of temperatures. Preliminary results showed that the sensor had a relatively high sensitivity to NO at 450 C and 1 V. NO concentrations from ppm to ppb ranges were detected with the low limit of near 159 ppb. Lower NO concentrations are being tested. Two sensing mechanisms were involved in the NO gas detection at ppm level: adsorption and oxidation reactions, whereas at ppb level of NO, only one sensing mechanism of adsorption was involved. The NO microsensor has the advantages of high sensitivity, small size, simple batch fabrication, high sensor yield, low cost, and low power consumption due to its microsize. The resistor-based thin-film sensor is meant for detection of low concentrations of NO gas, mainly in the ppb or lower range, and is being developed concurrently with other sensor technology for multispecies detection. This development demonstrates that ITO is a sensitive sensing material for NO detection. It also provides crucial information for future selection of nanostructured and nanosized NO sensing materials, which are expected to be more sensitive and to consume less power.

Abstract - Biochemical sensors for continuous monitoring require dependable periodic self- diagnosis with acceptable simplicity to check its functionality during operation. An in situ self- diagnostic technique for a dissolved oxygen microsensor is proposed in an effort to devise an intelligent microsensor system with an integrated electrochemical actuation electrode. With a built- in platinum microelectrode that surrounds the microsensor, two kinds of microenvironments, called the oxygen-saturated or oxygen-depleted phases, can be created by water electrolysis depending on the polarity. The functionality of the microsensor can be checked during these microenvironment phases. The polarographic oxygen microsensor is fabricated on a flexible polyimide substrate (Kapton) and the feasibility of the proposed concept is demonstrated in a physiological solution. The sensor responds properly during the oxygen-generating and oxygen- depleting phases. The use of these microenvironments for in situ self-calibration is discussed to achieve functional integration as well as structural integration of the microsensor system.

The capability to detect multianalyte ions in their mixed solution is an important advantage of voltammetry with an ionophore-based polymeric membrane against the potentiometric and optical counterparts. This advanced capability is highly attractive for the analysis of physiological ions at millimolar concentrations in biological and biomedical samples. Herein, we report on the comprehensive response mechanisms based on the voltammetric exchange and transfer of millimolar multiions at a thin polymeric membrane, where an ionophore is exhaustively depleted upon the transfer of the most favorable primary ion, I(zI). With a new voltammetric ion-exchange mechanism, the primary ion is exchanged with the secondary favorable ion, J(zJ), at more extreme potentials to transfer a net charge of |zJ|/nJ - |zI|/nI for each ionophore molecule, which forms 1:nI and 1:nJ complexes with the respective ions. Alternatively, an ion-transfer mechanism utilizes the second ionophore that independently transfers the secondary ion without ion exchange. Experimentally, a membrane is doped with a Na(+)- or Li(+)-selective ionophore to detect not only the primary ion, but also the secondary alkaline earth ion, based on the ion-exchange mechanism, where both ions form 1:1 complexes with the ionophores to transfer a net charge of +1. Interestingly, the resultant peak potentials of the secondary divalent ion vary with its sample activity to yield an apparently super-Nernstian slope as predicted theoretically. By contrast, the voltammetric exchange of calcium ion (nI = 3) with lithium ion (nJ = 1) by a Ca(2+)-selective ionophore is thermodynamically unfavorable, thereby requiring a Li(+)-selective ionophore for the ion-transfer mechanism. PMID:27111277

Voltammetric scanning electrochemical cell microscopy (SECCM) incorporates cyclic voltammetry measurements in the SECCM imaging protocol, by recording electrochemical currents in a wide potential window at each pixel in a map. This provides much more information compared to traditional fixed potential imaging. Data can be represented as movies (hundreds of frames) of current (over a surface region) at a series of potentials and are highly revealing of subtle variations in electrode activity. Furthermore, by combining SECCM data with other forms of microscopy, e.g. scanning electron microscopy and electron backscatter diffraction data, it is possible to directly relate the current-voltage characteristics to spatial position and surface structure. In this work we use a "hopping mode", where the SECCM pipet probe is translated toward the surface at a series of positions until meniscus contact. Small amounts of residue left on the surface, upon probe retraction, demark the precise area of each measurement. We use these techniques to study hydrazine oxidation on a polycrystalline platinum substrate both in air and in a deaerated environment. In both cases, the detected faradaic current shows a structural dependence on the surface crystallographic orientation. Significantly, in the presence of oxygen (aerated solution) the electrochemical current decreases strongly for almost all grains (crystallographic orientations). The results highlight the flexibility of voltammetric SECCM for electrochemical imaging and present important implications for hydrazine electroanalysis. PMID:25942527

Microsensors are powerful tools for microenvironment studies, however their use has often been restricted to laboratory applications due to the lack of adequate equipment for in situ deployments. Here we report on new features, construction details, and examples of applications of an improved diver-operated motorized microsensor profiler for underwater field operation to a water depth of 25 m. The new motorized profiler has a final precision of 5 microm, and can accommodate amperometric Clark-type microsensors for oxygen and hydrogen sulfide, potentiometric microsensors (e.g., for pH, Ca2+), and fiber-optic irradiance microsensors. The profiler is interfaced by a logger with a signal display, and has pushbuttons for underwater operation. The system can be pre-programmed to autonomous operation or interactively operated by divers. Internal batteries supply power for up to 24 h of measurements and 36 h of data storage (max. 64 million data points). Two flexible stands were developed for deployment on uneven or fragile surfaces, such as coral reefs. Three experimental pilot studies are presented, where (1) the oxygen distribution in a sand ripple was 3-D-mapped, (2) the microenvironment of sediment accumulated on a stony coral was studied, and (3) oxygen dynamics during an experimental sedimentation were investigated. This system allows SCUBA divers to perform a wide array of in situ measurements, with deployment precision and duration similar to those possible in the laboratory. PMID:17937304

We report fabrication and characterization of a new hydrogel-based microsensor for wireless chemical monitoring. The basic device structure is a high-sensitivity capacitive pressure sensor coupled to a stimuli-sensitive hydrogel that is confined between a stiff porous membrane and a thin glass diaphragm. As small molecules pass through the porous membrane, the hydrogel swells and deflects the diaphragm which is also the movable plate of the variable capacitor in an LC resonator. The resulting change in resonant frequency can be remotely detected by the phase-dip technique. Prior to hydrogel loading, the sensitivity of the pressure sensor to applied air pressure was measured to be 222 kHz/kPa over the range of 41.9-51.1 MHz. With a pH-sensitive hydrogel, the sensor displayed a sensitivity of 1.16 MHz/pH for pH 3.0-6.5, and a response time of 45 minutes. PMID:18335316

We propose an optical detection technique for liquid-crystal-based sensors that is based on polarization-resolved tracking of optical singularities and does not rely on standard observation of light-intensity changes caused by modifications of the liquid crystal orientational ordering. It uses a natural two-dimensional network of polarization singularities embedded in the transverse cross section of a probe beam that passes through a liquid crystal sample, in our case, a nematic droplet held in laser tweezers. The identification and spatial evolution of such a topological fingerprint is retrieved from subwavelength polarization-resolved imaging, and the mechanical constraint exerted on the molecular ordering by the trapping beam itself is chosen as the control parameter. By restricting our analysis to one type of point singularity, C points, which correspond to location in space where the polarization azimuth is undefined, we show that polarization singularities appear as intangible pointlike tracers for liquid-crystal-based three-dimensional microsensors. The method has a superresolution potential and can be used to visualize changes at the nanoscale.

The Micro Sensor System (MSS) is a layered sensor network with the goal of detecting dismounted threats approaching high value assets. A low power unattended ground sensor network is dependant on a network protocol for efficiency in order to minimize data transmissions after network establishment. The reduction of network 'chattiness' is a primary driver for minimizing power consumption and is a factor in establishing a low probability of detection and interception. The MSS has developed a unique protocol to meet these challenges. Unattended ground sensor systems are most likely dependant on batteries for power which due to size determines the ability of the sensor to be concealed after placement. To minimize power requirements, overcome size limitations, and maintain a low system cost the MSS utilizes advanced manufacturing processes know as Fluidic Self-Assembly and Chip Scale Packaging. The type of sensing element and the ability to sense various phenomenologies (particularly magnetic) at ranges greater than a few meters limits the effectiveness of a system. The MicroSensor System will overcome these limitations by deploying large numbers of low cost sensors, which is made possible by the advanced manufacturing process used in production of the sensors. The MSS program will provide unprecedented levels of real-time battlefield information which greatly enhances combat situational awareness when integrated with the existing Command, Control, Communications, Computers, Intelligence, Surveillance and Reconnaissance (C4ISR) infrastructure. This system will provide an important boost to realizing the information dominant, network-centric objective of Joint Vision 2020.

This paper presents the fabrication and characterization of a resonant pressure microsensor based on SOI-glass wafer-level vacuum packaging. The SOI-based pressure microsensor consists of a pressure-sensitive diaphragm at the handle layer and two lateral resonators (electrostatic excitation and capacitive detection) on the device layer as a differential setup. The resonators were vacuum packaged with a glass cap using anodic bonding and the wire interconnection was realized using a mask-free electrochemical etching approach by selectively patterning an Au film on highly topographic surfaces. The fabricated resonant pressure microsensor with dual resonators was characterized in a systematic manner, producing a quality factor higher than 10,000 (~6 months), a sensitivity of about 166 Hz/kPa and a reduced nonlinear error of 0.033% F.S. Based on the differential output, the sensitivity was increased to two times and the temperature-caused frequency drift was decreased to 25%. PMID:26402679

This paper presents the fabrication and characterization of a resonant pressure microsensor based on SOI-glass wafer-level vacuum packaging. The SOI-based pressure microsensor consists of a pressure-sensitive diaphragm at the handle layer and two lateral resonators (electrostatic excitation and capacitive detection) on the device layer as a differential setup. The resonators were vacuum packaged with a glass cap using anodic bonding and the wire interconnection was realized using a mask-free electrochemical etching approach by selectively patterning an Au film on highly topographic surfaces. The fabricated resonant pressure microsensor with dual resonators was characterized in a systematic manner, producing a quality factor higher than 10,000 (~6 months), a sensitivity of about 166 Hz/kPa and a reduced nonlinear error of 0.033% F.S. Based on the differential output, the sensitivity was increased to two times and the temperature-caused frequency drift was decreased to 25%. PMID:26402679

We describe the application of thin-film optical fibre Fabry-Perot (FFP) microsensors to high-bandwidth measurement of unsteady total temperature in transonic gas flows. An aerodynamic probe containing two temperature sensitive FFP microsensors was deployed in the rotor exit flow region of a gas turbine research rig. Measurements reveal gas temperature oscillations typically 4 K peak to peak at the blade passing frequency of 10 kHz with components to the third harmonic detected in the power spectrum of the temperature signal.

FET based microsensors have reached increasing importance in biomedical and environmental applications, due to their advantages over conventional sensors. These advantages are related with their small size, robustness, low cost, integrability, fast response time, and the small sample volumes required for their use. In this work, it is presented the design and implementation of a portable instrumentation system based on the CY8C29466 (PSoC) microcontroller for the measurement of ISFETs and CHEMFETs type microsensors in liquid samples. The system shows the measurement's data on a display, also allowing storage of data for further analysis by coupling the system to a PC serial port.

Presently, very few inexpensive technologies exist in the marketplace that can determine the contents of tank waste or monitor the chemistry of tank constituents in near-real time. The research addressed this problem by developing and assessing ceramic-metallic based microsensors for determining the constituents of a liquid organic storage tank by examining the gases in the headspace of the tank. Overall, the WBO and YSZ sensors responded well to the chemicals in this study. Responses to various concentrations were distinguishable visually. This is a clear indication that pattern recognition tools will be effective in resolving the constituents and concentrations. In tests, such as the test with acetophenone, one sensor, the WBO sensor is not extremely effective. However, the other sensor, the YSZ sensor, is effective in resolving the concentrations. This supports the need to use an array of sensors, as one sensor may be reactive to a compound while another may not. In the course of this research, several interesting phenomena surfaced. New sensors, that were fabricated but not used in a contaminant gas, seemed to function more effectively and predictably if a ?conditioning? step was imposed upon them prior to use in square wave voltammetry. A conditioning step consists of running cyclic voltammetry prior to running square wave voltammetry. This step tends to ?cleanse? the sensor surface by providing a full -1.0 V to +1.0V sweep and both oxidizing and reducing compounds on the sensor surface. [Note: squarewave voltammetry will simply oxidize or reduce compounds ? it will not induce both reactions.] This sweep is essential for recovery between samples.

Significant advances have recently been made to develop optically interrogated microsensor based chemical sensors with specific application to hydrogen vapor sensing and leak detection in the hydrogen economy. We have developed functionalized polymer-film and palladium/silver alloy coated microcantilever arrays with nanomechanical sensing for this application. The uniqueness of this approach is in the use of independent component analysis (ICA) and the classification techniques of neural networks to analyze the signals produced by an array of microcantilever sensors. This analysis identifies and quantifies the amount of hydrogen and other trace gases physisorbed on the arrays. Selectivity is achieved by using arrays of functionalized sensors with a moderate distribution of specificity among the sensing elements. The device consists of an array of beam-shaped transducers with molecular recognition phases (MRPs) applied to one surface of the transducers. Bending moments on the individual transducers can be detected by illuminating them with a laser or an LED and then reading the reflected light with an optical position sensitive detector (PSD) such as a CCD. Judicious selection of MRPs for the array provides multiple isolated interaction surfaces for sensing the environment. When a particular chemical agent binds to a transducer, the effective surface stresses of its modified and uncoated sides change unequally and the transducer begins to bend. The extent of bending depends upon the specific interactions between the microcantilever's MRP and the analyte. Thus, the readout of a multi-MRP array is a complex multidimensional signal that can be analyzed to deconvolve a multicomponent gas mixture. The use of this sensing and analysis technique in unattended networked arrays of sensors for various monitoring and surveillance applications is discussed.

This work describes the development of flexible, miniature and inexpensive nitrate sensors by electropolymerizing pyrrole onto carbon fiber substrates, using nitrate as a dopant. Carbon microfibers were found to be an excellent substitute to expensive conductive materials, such as glassy carbon or platinum. The electrodes with a 3-5 micron layer of NO3 -doped polypyrrole (PPy) exhibited a promising lifetime (at least 2 month without changes in sensitivity and linear response), fast response times (seconds), and sensitivity competitive to commercial nitrate ISE. Nernstian sensor response slopes of 54 to 58 mV/(decade concentration) for single filament have been observed, with a linear response to nitrate concentrations spanning three orders of magnitude (0.1 - 10-4 M or 6200 - 6.2 ppm of NO3-), and a detection limit of (3 ± 1) x 10-5 M (1.25-2.5 ppm). An advantage of using the carbon fibers as a substrate for pyrrole polymerization process is that these fibers are relatively easy to manipulate, lending themselves to root-like electrode designs which may be ideal for observing the water chemistry of soil moisture. Using prototypical PPy-coated microfibers, we have been able to directly measure nitrate concentrations in residual soil water contents as low as 8 percent by weight for a medium sand. Results for model soils and field samples are presented in which direct measurements with the microsensors compare reasonably well with a more conventional analytical method entailing soil extraction and analysis by the Griess-Romijn method.

Improved in-situ meteorological measurements are needed for monitoring the weather and climate of the terrestrial and Martian atmospheres. We have initiated a program to assess the feasibility and utility of micro-sensors for precise in-situ meteorological measurements in these environments. Sensors are being developed for measuring pressure, temperature, wind velocity, humidity, and aerosol amounts. Silicon micro-machining and large scale integration technologies are being used to make sensors that are small, rugged, lightweight, and require very little power. Our long-term goal is to develop very accurate miniaturized sensors that can be incorporated into complete instrument packages or 'micro weather stations,' and deployed on a variety of platforms. If conventional commercially available silicon production techniques can be used to fabricate these sensor packages, it will eventually be possible to mass-produce them at low cost. For studies of the Earth's troposphere and stratosphere, they could be deployed on aircraft, dropsondes, radiosondes, or autonomous surface stations at remote sites. Improved sensor accuracy and reduced sensor cost are the primary challenges for these applications. For studies of the Martian atmosphere, these sensor packages could be incorporated into the small entry probes and surface landers that are being planned for the Mars Environmental SURvey (MESUR) Mission. That decade-long program will deploy a global network of small stations on the Martian surface for monitoring meteorological and geological processes. Low mass, low power, durability, large dynamic range and calibration stability are the principal challenges for this application. Our progress on each of these sensor types is presented.

A real-time, labeled-free and nanogram-sensitive mass sensor, electrochemical quartz crystal microbalance (EQCM) is used to monitor a cyclic voltammetric deposition of polyaniline (PANI). The results determined that the efficiency for PANI deposition and the anion-doping ratio is calculated in one single cyclic voltammetric.

Staircase voltammetric stripping is an attractive alternative to both differential pulse and linear scan voltammetric stripping. This paper presents a theoretical treatment of this new stripping mode applied to the thin-film mercury electrode. For equivalent scan rates the faradaic response is somewhat smaller than that obtained by linear scan stripping.

Biofilms have been implicated in delayed wound healing, although the mechanisms by which biofilms impair wound healing are poorly understood. Many species of bacteria produce exotoxins and exoenzymes that may inhibit healing. In addition, oxygen consumption by biofilms and by the responding leukocytes, may impede wound healing by depleting the oxygen that is required for healing. In this study, oxygen microsensors to measure oxygen transects through in vitro cultured biofilms, biofilms formed in vivo within scabs from a diabetic (db/db) mouse wound model, and ex vivo human chronic wound specimens was used. The results showed that oxygen levels within mouse scabs had steep gradients that reached minima ranging from 17 to 72 mmHg on live mice and from 6.4 to 1.1 mmHg on euthanized mice. The oxygen gradients in the mouse scabs were similar to those observed for clinical isolates cultured in vitro and for human ex vivo specimens. To characterize the metabolic activities of the bacteria in the mouse scabs, transcriptomics analyses of Pseudomonas aeruginosa biofilms associated with the db/db mice wounds was performed. The results demonstrated that the bacteria expressed genes for metabolic activities associated with cell growth. Interestingly, the transcriptome results also indicated that the bacteria within the wounds experienced oxygen-limitation stress. Among the bacterial genes that were expressed in vivo were genes associated with the Anr-mediated hypoxia-stress response. Other bacterial stress response genes highly expressed in vivo were genes associated with stationary-phase growth, osmotic stress, and RpoH-mediated heat shock stress. Overall, the results supported the hypothesis that bacterial biofilms in chronic wounds promote chronicity by contributing to the maintenance of localized low oxygen tensions, through their metabolic activities and through their recruitment of cells that consume oxygen for host defensive processes. PMID:26748963

A voltammetric determination of possible organic pollutants such as diol and phenolic compounds in water was studied using ferroceneboronic acid (FBA) as a redox-active marker. A cyclic voltammogram of FBA exhibited a pair of oxidation and reduction peaks at 230 and 170 mV at pH 7.0, respectively, while another pair of redox peaks was observed in the presence of diol or phenolic compounds tested. The results were rationalized based on the formation of boronate esters of FBA with the added compounds. The changes in the redox peak currents were dependent on the concentration of the additives, suggesting a usefulness of FBA in the electrochemical determination of these compounds in water. PMID:22066227

The electrochemical behaviour of several N-containing voltammetricactive drugs such as 1,4-benzodiazepines (chlordiazepoxide, nitrazepam and diazepam) as well as one nitro-compound (nitrofurantoin) and one azo-compound (phenazopyridine) is described using a new kind of liquid electrode, the hanging galinstan drop electrode. Concentrations of 10(-5) - 10(-8) mol L(-1) are generally measurable. Differential pulse and adsorptive stripping voltammograms are recorded in different supporting electrolytes, like 0.1 M KNO3, acetate buffer solution pH = 4.6 and phosphate buffer solution pH = 7.0. The effects of varying the starting potentials, U(start) for DPV and accumulation times, t(acc) for AdSV are considered. Briefly, it is shown that the novel galinstan electrode is suitable for reducing several functional groups in organic substances, here presented for N-oxide-, azomethine-, nitro- and azo-groups. PMID:19348337

Control of oxygen and water in the root zone is vital to support plant growth in the microgravity environment. The ability to control these sometimes opposing parameters in the root zone is dependent upon the availability of sensors to detect these elements and provide feedback for control systems. In the present study we demonstrate the feasibility of using microsensor arrays on a flexible substrate for dissolved oxygen detection, and a 4-point impedance microprobe for surface wetness detection on the surface of a porous tube (PT) nutrient delivery system. The oxygen microsensor reported surface oxygen concentrations that correlated with the oxygen concentrations of the solution inside the PT when operated at positive pressures. At negative pressures the microsensor shows convergence to zero saturation (2.2 micro mol/L) values due to inadequate water film formation on porous tube surface. The 4-point microprobe is useful as a wetness detector as it provides a clear differentiation between dry and wet surfaces. The unique features of the dissolved oxygen microsensor array and 4-point microprobe include small and simple design, flexibility and multipoint sensing. The demonstrated technology is anticipated to provide low cost, and highly reliable sensor feedback monitoring plant growth nutrient delivery system in both terrestrial and microgravity environments.

Monitoring phosphate concentration is very important to prevent and control eutrophication in natural waters. In this study, cobalt-based microsensors were modified, characterized, and tested to monitor internal soluble phosphorous (SRP) loading in lakes with improved detection limits. The effectiveness of surface modification on the performance of a cobalt-based microelectrode was fully examined by determining detection limit, response time, selectivity, interference with ions (sulfate, nitrate, and nitrite) and dissolved oxygen (DO). To assess their performance, phosphate sensors were applied to sediment samples collected from Lake Erie. SRP loading from sediments was determined under different DO conditions. After increasing the phosphate sensing area and modifying the surface, phosphate microsensors showed an increased detection limit of up to 10(-8) M concentration of phosphate ion. The phosphate microsensor also showed its ability to measure sediment SRP profiling without disturbing sediment structure, and diffusion coefficients of phosphate in sediment could be determined under both oxic and anoxic conditions. Modified phosphate sensors showed improved sensitivity and could be applied to both water and sediment samples with high spatial resolution; however, signal interferences (especially with oxygen) required consideration during sample analysis. Overall, obtained results showed that phosphate microsensors can be an effective tool for measurement of phosphate in lake water and sediment samples for SRP monitoring. PMID:26156193

Microsensors and Microelectromechanical Systems (MEMS) are currently being applied to the structural health monitoring of critical aircraft components. The approach integrates acoustic emission, strain gauges, MEMS accelerometers and vibration monitoring devices with signal processing electronics to provide real-time indicators of incipient failure of aircraft components with a known history of catastrophic failure due to fracture.

A first step towards the fabrication and electrochemical evaluation of thin-film microsensors based on organic PVC membranes for the determination of Hg(II), Cd(II), Pb(II) and Cu(II) ions in solutions has been realised. The membrane-coating mixture used in the preparation of this new type of microsensors is incorporating PVC as supporting matrix, o-nitrophenyloctylether (o-NPOE) as solvent mediator and a recently synthesized Hg[dimethylglyoxime(phene)]2+ and Bis-(4-hydroxyacetophenone)-ethylenediamine as electroactive materials for Hg(II) and Cd(II), respectively. A set of three commercialised ionophores for Cd(II), Pb(II) and Cu(II) has been also used for comparison. Thin-film microsensors based on these membranes showed a Nernstian response of slope (26-30 mV/dec.) for the respective tested cations. The potentiometric response characteristics (linear range, pH range, detection limit and response time) are comparable with those obtained by conventional membranes as well as coated wire electrodes prepared from the same membrane. The realisation of the new organic membrane-based thin-film microsensors overcomes the problem of an insufficient selectivity of solid-state-based thin-film sensors.

Microsensing is a leading field in technology due to its wide application potential, not only in bio-engineering, but in other fields as well. Microsensors have potentially low-cost manufacturing processes, while a single device type can have various uses, and this consequently helps with the ever-growing need to provide better health conditions in rural parts of the world. Capacitive biosensors detect a change in permittivity (or dielectric constant) of a biological material, usually within a parallel plate capacitor structure which is often implemented with integrated electrodes of an inert metal such as gold or platinum on a microfluidic substrate typically with high dielectric constant. There exist parasitic capacitance components in these capacitive sensors, which have large influence on the capacitive measurement. Therefore, they should be considered for the development of sensitive and accurate sensing devices. An analytical model of a capacitive sensor device is discussed, which accounts for these parasitic factors. The model is validated with a laboratory device of fixed geometry, consisting of two parallel gold electrodes on an alumina (Al2O3) substrate mounted on a glass microscope slide, and with a windowed cover layer of poly-dimethyl-siloxane (PDMS). The thickness of the gold layer is 1μm and the electrode spacing is 300μm. The alumina substrate has a thickness of 200μm, and the high relative permittivity of 11.5 is expected to be a significantly contributing factor to the total device capacitance. The 155μm thick PDMS layer is also expected to contribute substantially to the total device capacitance since the relative permittivity for PDMS is 2.7. The wideband impedance analyser evaluation of the laboratory device gives a measurement result of 2pF, which coincides with the model results; while the handheld RLC meter readout of 4pF at a frequency of 10kHz is acceptable within the measurement accuracy of the instrument. This validated model will

Tissue oxygenation is a key factor ensuring normal tissue functions and viability. Continuous real-time monitoring of the partial pressure of oxygen, pO(2), in tissues gives insight into the dynamic fluctuations of O(2) supplies to tissues by blood circulation. Small oxygen sensors enable investigations of the spatial variation of pO(2) in tissues at different locations in relation to local microvessels. In this paper, pO(2) measurement using microelectrodes and biocompatible sensorsv is discussed and recent progress of their application in human skin is reviewed. Emphasis is given to working principles of a number of existing oxygen sensors and their potential application in vivo and in tissue engineering. Results on spatial and temporal variations of the pO(2) in human skin introduced by localized ischaemia-reperfusion are presented when the surface of the skin is covered by an oxygen-free paraffin oil layer and the range of the tissue pO(2) is deduced to be between 0 and 60 mmHg. In the study, pO(2) increases from 8.0 +/- 3.2 mmHg (n = 6) at the surface of the skin to 35.2 +/- 8.0 mmHg (n = 9) at a depth just above the subpapillary plexus. Temporal decay in pO(2) following tissue compression and rise in pO(2) following pressure release can be described using mono-exponential functions. The time constant for the exponential decay, tau = 8.44 +/- 1.53 s (n = 7) is consistently greater than that for the exponential rises, tau' = 4.75 +/- 0.82 s (n = 6). The difference in pO2 change with the time following tissue compression and pressure release reveals different dynamic mechanisms involved in the two transient phases. The elevated steady state pO(2) following reperfusion, which is approximately 20% higher than the pre-occlusion value, indicates localized reactive hyperaemia. Possible applications of O(2) microsensors in diseases, e.g. tumours, pressure ulcers, are also discussed. PMID:16849157

Voltammetric detection of biological molecules was carried out using chopped carbon fibers produced from carbon fiber reinforced plastics that are biocompatible and inexpensive. Because chopped carbon fibers normally are covered with a sizing agent, they are difficult to use as an electrode. However, when the surface of a chopped carbon fiber was treated with ethanol and hydrochloric acid, it became conductive. To evaluate the functioning of chopped carbon fibers, voltammetric measurements of [Fe(CN)(6)](3-) were carried out. Redoxes of FAD, ascorbic acid and NADH as biomolecules were recorded using cyclic voltammetry. The sizing agents used to bundle the fibers were epoxy, polyamide and polyurethane resins. The peak currents were the greatest when using the chopped carbon fibers that were created with epoxy resins. When the electrode response of the chopped carbon fibers was compared with that of a glassy carbon electrode, the peak currents and the reversibility of the electrode reaction were sufficient. Therefore, the chopped carbon fibers will be useful as disposable electrodes for the sensing of biomolecules. PMID:20953048

At the potential range where both decamethylferrocene (dMeFc) and ferrocene (Fc) are oxidized with rates controlled by linear diffusion, electrogenerated Fc(+) radicals diffusing outwards from the electrode react quantitatively (K23 C=5.8 x 10(exp 8) with dMeFc diffusing towards the electrode and produce Fc and dMeFc. That reaction replaces dMeFc with Fc, whose diffusion coefficient is higher than that of dMeFc(+), and the total mass-transfer limited current from the mixture is increased by approximately 10%. Analogous observations are made when mass-transfer is controlled by convective-diffusion as in RDE voltammetry. Similar results have been obtained with another, and for all practical purposes randomly selected pair of redox-active substances, [Co(bipy)3](2+) and N - methylphenothiazine (MePTZ); reaction of MePTZ(+) with [Co(bipy)3](2+) replaces the latter with MePTZ, which diffuses faster and the current increases by approximately 20%. The experimental voltammograms have been simulated numerically and the role of (a) the rate constant of the homogeneous reaction; (b) the relative concentrations; and, (c) the diffusion coefficients of all species involved have been studied in detail. Importantly, it was also identified that within any given redox system the dependence of the mass-transfer limited current on the bulk concentrations of the redox-active species is expected to be non-linear. These findings are discussed in terms of their electroanalytical implications.

This work describes the single-use electrochemical DNA biosensor technology developed for voltammetric detection of sequence selective DNA hybridization related to important human and veterinary pathogen; Toxoplasma gondii. In the principle of electrochemical label-free detection assay, the duplex of DNA hybrid formation was detected by measuring guanine oxidation signal occured in the presence of DNA hybridization. The biosensor design consisted of the immobilization of an inosine-modified (guanine-free) probe onto the surface of pencil graphite electrode (PGE), and the detection of the duplex formation in connection with the differential pulse voltammetry(DPV) by measuring the guanine signal. Toxoplasma gondii capture probe was firstly immobilized onto the surface of the activated PGE by wet adsorption. The extent of hybridization at PGE surface between the probe and the target was then determined by measuring the guanine signal observed at +1.0V. The electrochemical monitoring of optimum DNA hybridization has been performed in the target concentration of 40µg/mL in 50min of hybridization time. The specificity of the electrochemical biosensor was then tested using non-complementary, or mismatch short DNA sequences. Under the optimum conditions, the guanine oxidation signal indicating full hybridization was measured in various target concentration from 0.5 to 25µg/mL and a detection limit was found to be 1.78µg/mL. This single-use biosensor platform was successfully applied for the voltammetric detection of DNA hybridization related to Toxoplasma gondii in PCR amplicons. PMID:26717837

The good composition and activity of biofilms are very important for successful operation and control of fixed-film biological reactors employed in liquid effluents treatment. During the last decade, microsensors have been applied to study microbial ecology. These sensors could provide information regarding the microbial activity concerning nitrification and denitrification that occur inside biofilms. Other techniques of molecular biology, such as fluorescence in situ hybridization (FISH), have also contributed to this matter because their application aids in the identification of the bacterial populations that compose the biofilms. The focus of this paper was to study the loading rate and surface velocity to promote the development of nitrifying biofilms in three distinct flow cells that were employed in the post treatment of a synthetic wastewater simulating the effluent from a UASB (Upflow Anaerobic Sludge Blanket) reactor. Using the FISH technique, it was found that the population of ammonia-oxidizing-bacteria was greater than that of nitrite-oxidizing-bacteria; this was also supported by the lower production of nitrate determined by physicochemical and microsensor analyses. It was verified that the loading rate and surface velocity that promoted the greatest nitrogen removal were 0.25 g N-amon m(-2)biofilm day(-1) and 1 m h(-1), respectively. PMID:22335102

Oxygen deficiency is commonplace in seeds, and limits both their development and their germination. It is, therefore, of considerable relevance to crop production. While the underlying physiological basis of seed hypoxia has been known for some time, the lack of any experimental means of measuring the global or localized oxygen concentration within the seed has hampered further progress in this research area. The development of oxygen-sensitive microsensors now offers the capability to determine the localized oxygen status within a seed, and to study its dynamic adjustment both to changes in the ambient environment, and to the seed's developmental stage. This review illustrates the use of oxygen microsensors in seed research, and presents an overview of existing data with an emphasis on crop species. Oxygen maps, both static and dynamic, should serve to increase our basic understanding of seed physiology, as well as to facilitate upcoming breeding and biotechnology-based approaches for crop improvement. PMID:22412307

Measuring temperature is an extensively explored field of analysis, but measuring a temperature change in a nanoparticle is a new challenge. Here, a microsensor is configured to measure temperature changes in gold nanorods in solution upon laser irradiation. The device consists of a silicon wafer coated with silicon nitride in which a microfabricated resistance temperature detector was embedded and attached to a digital multimeter. A polydimethylsiloxane mold served as a microcontainer for the sample attached on top of the silicon membrane. This enables laser irradiation of the gold nanorods and subsequent measurement of temperature changes. The results showed a temperature increase of 8 to 10 °C and good correlation with theoretical calculations and bulk sample direct temperature measurements. These results demonstrate the suitability of this simple temperature microsensor for determining laser-induced heating profiles of metallic nanomaterials; such measurements will be essential for optimizing therapeutic and catalytic applications. PMID:25303932

Designing a micro, high reliability weak signal extracting system is a critical problem need to be solved in the application of silicon resonant micro-sensor. The closed-loop testing system based on FPGA uses software to replace hardware circuit which dramatically decrease the system's mass and power consumption and make the system more compact, both correlation theory and frequency scanning scheme are used in extracting weak signal, the adaptive frequency scanning arithmetic ensures the system real-time. The error model was analyzed to show the solution to enhance the system's measurement precision. The experiment results show that the closed-loop testing system based on FPGA has the personality of low power consumption, high precision, high-speed, real-time etc, and also the system is suitable for different kinds of Silicon Resonant Micro-sensor.

In this paper we investigate the fabrication process of a novel polymer based pressure micro-sensor for use in manometric measurements in medical diagnostics. Review and analysis of polymer materials properties and polymer based sensors has been carried out and has been reported by us elsewhere [1]. The interest in developing a novel polymer based flexible pressure micro-sensor was motivated by the numerous problems inherent in the currently available manometric catheters used in the hospitals. The most critical issue regarding existing catheters was the running and maintenance costs [2]. Thus expensive operation costs lead to reuse of the catheters, which increase the risk for disease transmission. The novel flexible polymer based pressure micro-sensor was build using SU-8, which is a special kind of negative photoresist. Single-walled carbon nanotubes (SWCNTs) and aluminum are used as the sensing material and contacting electrodes respectively. The pressure sensor diaphragm was first patterned on top of an oxidized silicon wafer using SU-8, followed by aluminum deposition to define the electrodes. The carbon nanotube is then deposited using dielectrophoresis (DEP) process. Once the carbon nanotubes are aligned in between these electrodes, the remaining of the sensor structure is formed using SU-8. Patterning of SU-8 and release from the substrate make the device ready for further testing of sensing ability. This research not only investigates the use of polymeric materials to build pressure sensors, but also explores the feasibility of full utilization of polymeric materials to replace conventional silicon materials in micro-sensors fabrication for use in medical environments. The completed sensor is expected to form an integral part of a large versatile sensing system. For example, the biocompatible artificial skin, is predicted to be capable of sensing force, pressure, temperature, and humidity, and may be used in such applications as medical and robotic system.

Cerebral blood flow (CBF) plays a critical role in the exchange of nutrients and metabolites at the capillary level and is tightly regulated to meet the metabolic demands of the brain. After major brain injuries, CBF normally decreases and supporting the injured brain with adequate CBF is a mainstay of therapy after traumatic brain injury. Quantitative and localized measurement of CBF is therefore critically important for evaluation of treatment efficacy and also for understanding of cerebral pathophysiology. We present here an improved thermal flow microsensor and its operation which provides higher accuracy compared to existing devices. The flow microsensor consists of three components, two stacked-up thin film resistive elements serving as composite heater/temperature sensor and one remote resistive element for environmental temperature compensation. It operates in constant-temperature mode (~2 °C above the medium temperature) providing 20 ms temporal resolution. Compared to previous thermal flow microsensor based on self-heating and self-sensing design, the sensor presented provides at least two-fold improvement in accuracy in the range from 0 to 200 ml/100 g/min. This is mainly achieved by using the stacked-up structure, where the heating and sensing are separated to improve the temperature measurement accuracy by minimization of errors introduced by self-heating. PMID:26256480

An integrated multifunction micro-sensor for three-dimensional micro-force precision measurement under different pressure and temperature conditions is introduced in this paper. The integrated sensor consists of three kinds of sensors: a three-dimensional micro-force sensor, an absolute pressure sensor and a temperature sensor. The integrated multifunction micro-sensor is fabricated on silicon wafers by micromachining technology. Different doping doses of boron ion, placement and structure of resistors are tested for the force sensor, pressure sensor and temperature sensor to minimize the cross interference and optimize the properties. A glass optical fiber, with a ladder structure and sharp tip etched by buffer oxide etch solution, is glued on the micro-force sensor chip as the tactile probe. Experimental results show that the minimum force that can be detected by the force sensor is 300 nN; the lateral sensitivity of the force sensor is 0.4582 mV/μN; the probe length is linearly proportional to sensitivity of the micro-force sensor in lateral; the sensitivity of the pressure sensor is 0.11 mv/KPa; the sensitivity of the temperature sensor is 5.836 × 10−3 KΩ/°C. Thus it is a cost-effective method to fabricate integrated multifunction micro-sensors with different measurement ranges that could be used in many fields. PMID:22666017

The major limiting factor in kidney clinical transplantation is the shortage of transplantable organs. The current inability to distinguish viability from non-viability on a prospective basis represents a major obstacle in any attempt to expand organ donor criteria. Consequently, a way to measure and monitor a relevant analyte to assess kidney viability is needed. For the first time, the initial development and characterization of a metabolic microsensor to assess kidney viability is presented. The rate of glucose consumption appears to serve as an indicator of kidney metabolism that may distinguish reversible from irreversible kidney damage. The proposed MetaSense (Metabolic Sensor) microdevice would replace periodic laboratory diagnosis tests with a continuous monitor that provides real-time data on organ viability. Amperometry, a technique that correlates an electrical signal with analyte concentration, is used as a method to detect glucose concentrations. A novel two-electrode electrochemical sensing cell design is presented. It uses a modified metallic working electrode (WE) and a bare metallic reference electrode (RE) that acts as a pseudo-reference/counter electrode as well. The proposed microsensor has the potential to be used as a minimally invasive sensor for its reduced number of probes and very small dimensions achieved by micromachining and lithography. In order to improve selectivity of the microdevice, two electron transfer mechanisms or generations were explored. A first generation microsensor uses molecular oxygen as the electron acceptor in the enzymatic reaction and oxidizes hydrogen peroxide (H2O2) to get the electrical signal. The microsensor's modified WE with conductive polymer polypyrrole (PPy) and corresponding enzyme glucose oxidase (GOx) immobilized into its matrix, constitutes the electrochemical detection mechanism. Photoluminescence spectroscopic analysis confirmed and quantified enzyme immobilized concentrations within the matrix. In

Cleavage of amyloid precursor protein (APP) by the β-site APP cleaving enzyme 1 (BACE1) is a key step in the formation of amyloid beta (Aβ) peptide, the main component of amyloid plaques in Alzheimer's disease (AD). Suppression of BACE1 activity has thus become an efficient way for the treatment of AD. In this study, BACE1 in the absence or presence of BACE1 inhibitors was exposed to the biotinylated peptide substrate-modified electrode. This step was followed by the attachment of ferrocene (Fc)-capped gold nanoparticle/streptavidin conjugates. Due to the blockage of the BACE1 activity by select inhibitors, well-defined voltammetric peaks of high signal intensity were obtained. However, featureless voltammogram was obtained upon initiating the cleavage reaction. The proposed method is simple, sensitive, and suitable for monitoring of BACE1 activity and screening of BACE1 inhibitors. PMID:23867352

The high ion selectivity of potentiometric and optical sensors based on ionophore-based polymeric membranes is thermodynamically limited. Here, we report that the voltammetric selectivity of thin ionophore-based polymeric membranes can be kinetically improved by several orders of magnitude in comparison with their thermodynamic selectivity. The kinetic improvement of voltammetric selectivity is evaluated quantitatively by newly introducing a voltammetric selectivity coefficient in addition to a thermodynamic selectivity coefficient. Experimentally, both voltammetric and thermodynamic selectivity coefficients are determined from cyclic voltammograms of excess amounts of analyte and interfering ions with respect to the amount of a Na(+)- or Li(+)-selective ionophore in thin polymeric membranes. We reveal the slower ionophore-facilitated transfer of a smaller alkaline earth metal cation with higher hydrophilicity across the membrane/water interface, thereby kinetically improving voltammetric Na(+) selectivity against calcium, strontium, and barium ions by 3, 2, and 1 order of magnitude, respectively, in separate solutions. Remarkably, voltammetric Na(+) and Li(+) selectivity against calcium and magnesium ions in mixed solutions is improved by 4 and >7 orders of magnitude, respectively, owing to both thermodynamic and kinetic effects in comparison with thermodynamic selectivity in separate solutions. Advantageously, the simultaneous detection of sodium and calcium ions is enabled voltammetrically in contrast to the potentiometric and optical counterparts. Mechanistically, we propose a new hypothetical model that the slower transfer of a more hydrophilic ion is controlled by its partial dehydration during the formation of the adduct with a "water finger" prior to complexation with an ionophore at the membrane/water interface. PMID:27527590

The purpose of this study was to clarify the relationship between neuron cells and astrocyte cells in regulating glutamate toxicity on the 10th and 20th day in vitro. A mixed primary culture system from newborn rats that contain cerebral cortex neurons cells was employed to investigate the glutamate toxicity. All cultures were incubated with various glutamate concentrations, then viability tests and histological analyses were performed. The activities of glutamate transporters were determined by using in vitro voltammetry technique. Viable cell number was decreased significantly on the 10th day at 10(-7) M and at 10(-6) M glutamate applications, however, viable cell number was not decreased at 20th day. Astrocyte number was increased nearly six times on the 20th day as compared to the 10th day. The peak point of glutamate reuptake capacity was about 2 × 10(-4) M on the 10th day and 10(-3) M on the 20th day. According to our results, we suggested that astrocyte age was important to maintain neuronal survival against glutamate toxicity. Thus, we revealed activation or a trigger point of glutamate transporters on astrocytes due to time since more glutamate was taken up by astrocytes when glutamate transporters on the astrocyte were triggered with high exogenous glutamate concentrations. In conclusion, the present investigation is the first voltammetric study on the reuptake parameters of glutamate in vitro. PMID:26438331

In this work, a square-wave voltammetric method based on sulphite electrochemical reduction was developed for quantification of this preservative in commercial beverages. A carbon-paste electrode chemically modified with multiwalled carbon nanotubes was used as the working electrode. Under the optimised experimental conditions, a linear response to sulphite concentrations from 1.6 to 32 mg SO2 L(-1) (25-500 μmol L(-1) of sulphite), with a limit of detection of 1.0 mg SO2 L(-1) (16 μmol L(-1) of sulphite), was obtained. This method does not suffer interference from other common beverage additives such as ascorbic acid, fructose, and sucrose, and it enables fast and reliable sulphite determination in beverages, with minimal sample pretreatment. Despite its selectivity, the method is not applicable to red grape juice or red wine samples, because some of their components produce a cathodic peak at almost the same potential as that of sulphite reduction. PMID:25466087

This review discusses from a critical perspective the development of new sensors for the measurement of priority pollutants targeted in the E.U. Water Framework Directive. Significant advances are reported in the paper and their advantages and limitations are also discussed. Future perspectives in this area are also pointed out in the conclusions. This review covers publications appeared since December 2006 (the publication date of the Swift report). Among priority substances, sensors for monitoring the four WFD metals represent 81% of published papers. None of analyzed publications present a micro-sensor totally validated in laboratory, ready for tests under real conditions in the field. The researches are mainly focused on the sensing part of the micro-sensors. Nevertheless, the main factor limiting micro-sensor applications in the environment is the ruggedness of the receptor towards environmental conditions. This point constitutes the first technological obstacle to be overcome for any long-term field tests. PMID:22163635

Voltammetric sensors made with films of polyions, double-stranded DNA and liver microsomes adsorbed layer-by-layer onto pyrolytic graphite electrodes were evaluated for reactive metabolite screening. This approach features simple, inexpensive screening without enzyme purification for applications in drug or environmental chemical development. Cytochrome P450 enzymes (CYPs) in the liver microsomes were activated by an NADPH regenerating system or by electrolysis to metabolize model carcinogenic compounds nitrosamine and styrene. Reactive metabolites formed in the films were trapped as adducts with nucleobases on DNA. The DNA damage was detected by square-wave voltammetry (SWV) using Ru(bpy)32+ as a DNA-oxidation catalyst. These sensors showed a larger rate of increase in signal vs. reaction time for a highly toxic nitrosamine than for the moderately toxic styrene due to more rapid reactive metabolite-DNA adduct formation. Results were consistent with reported in vivo TD50 data for the formation of liver tumors in rats. Analogous polyion/ liver microsome films prepared on 500 nm silica nanoparticles (nanoreactors) and reacted with nitrosamine or styrene, provided LC-MS or GC analyses of metabolite formation rates that correlated well with sensor response. PMID:23100998

The preparation and application of a practical electrochemical sensor for environmental monitoring and assessment of heavy metal ions in samples is a subject of considerable interest. In this paper, a carbon paste electrode modified with maize tassel for the determination of Cu(II) has been proposed. Scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) were used to study morphology and identify the functional groups on the modified electrode, respectively. First, Cu(II) was adsorbed on the carbon paste electrode surface at open circuit and voltammetric techniques were used to investigate the electrochemical performances of the sensor. The electrochemical sensor showed an excellent electrocatalytic activity towards Cu(II) at pH 5.0 and by increasing the amount of maize tassel biomass, a maximum response at 1:2.5 (maize tassel:carbon paste; w/w) was obtained. The electrocatalytic redox current of Cu(II) showed a linear response in the range (1.23 μM to 0.4 mM) with the correlation coefficient of 0.9980. The limit of detection and current-concentration sensitivity were calculated to be 0.13 (±0.01) μM and 0.012 (±0.001) μA/μM, respectively. The sensor gave good recovery of Cu(II) in the range from 96.0 to 98.0 % when applied to water samples. PMID:24705875

A voltammetric biosensor based on tyrosinase (TYR) was developed for determination of tyramine. Carbon material (multi-walled carbon nanotubes or mesoporous carbon CMK-3-type), polycationic polymer-i.e., poly(diallyldimethylammonium chloride) (PDDA), and Nafion were incorporated into titania dioxide sol (TiO2) to create an immobilization matrix. The features of the formed matrix were studied by scanning electron microscopy (SEM) and cyclic voltammetry (CV). The analytical performance of the developed biosensor was evaluated with respect to linear range, sensitivity, limit of detection, long-term stability, repeatability, and reproducibility. The biosensor exhibited electrocatalytic activity toward tyramine oxidation within a linear range from 6 to 130 μM, high sensitivity of 486 μA mM(-1) cm(-2), and limit of detection of 1.5 μM. The apparent Michaelis-Menten constant was calculated to be 66.0 μM indicating a high biological affinity of the developed biosensor for tyramine. Furthermore, its usefulness in determination of tyramine in food product samples was also verified. Graphical abstract Different food samples were analyzed to determine tyramine using biosensor based on tyrosinase. PMID:27209590

As a core component for open-loop characteristics testing system of micro-sensor, quality of signal source influences the integer performances of testing system directly. The method to generate special signal of open-loop testing system of resonant micro-sensor are discussed in this paper, and a method of direct digital frequency synthesize (DDS) to develop the special signal source of the testing system is proposed. A designation approach based on DSP and FPGA in the realization of DDS is advocated. Finally a simulation is made using the MATLAB. The principle of DDS is also introduced.

5-Hydroxytryptamine (5-HT) is an important molecule in the brain that is implicated in mood and emotional processes. In vivo, its dynamic release and uptake kinetics are poorly understood due to a lack of analytical techniques for its rapid measurement. Whereas fast-scan cyclic voltammetry with carbon fiber microelectrodes is used frequently to monitor subsecond dopamine release in freely moving and anesthetized rats, the electrooxidation of 5-HT forms products that quickly polymerize and irreversibly coat the carbon electrode surface. Previously described modifications of the electrochemical waveform allow stable and sensitive 5-HT measurements in mammalian tissue slice preparations and in the brain of fruit fly larvae. For in vivo applications in mammals, however, the problem of electrode deterioration persists. We identify the root of this problem to be fouling by extracellular metabolites such as 5-hydoxyindole acetic acid (5-HIAA), which is present in 200-1000 times the concentration of 5-HT and displays similar electrochemical properties, including filming of the electrode surface. To impede access of the 5-HIAA to the electrode surface, a thin layer of Nafion, a cation exchange polymer, has been electrodeposited onto cylindrical carbon-fiber microelectrodes. The presence of the Nafion film was confirmed with environmental scanning electron microscopy and was demonstrated by the diminution of the voltammetric signals for 5-HIAA as well as other common anionic species. The modified microelectrodes also display increased sensitivity to 5-HT, yielding a characteristic cyclic voltammogram that is easily distinguishable from other common electroactive brain species. The thickness of the Nafion coating and a diffusion coefficient (D) in the film for 5-HT were evaluated by measuring permeation through Nafion. In vivo, we used physiological, anatomical, and pharmacological evidence to validate the signal as 5-HT. Using Nafion-modified microelectrodes, we present the

Electroreduction and adsorption of cefixime was studied in phosphate buffer by cyclic voltammetry (CV), differential pulse cathodic adsorptive stripping voltammetry (DPCAdSV), and square-wave cathodic adsorptive stripping voltammetry (SWCAdSV) at hanging mercury drop electrode (HMDE). These fully validated sensitive and reproducible cathodic adsorptive stripping voltammetric procedures were applied for the trace determination of the bulk drug in pharmaceutical formulations and in human urine. The optimal experimental parameters were as follows: accumulation potential=-0.1 V (vs. Ag/AgCl, 3M KCl), accumulation time=50s, frequency=140 Hz, pulse amplitude=0.07 V, and scan increment=10 mV in phosphate buffer (pH 2.6). The first peak current showed a linear dependence with the drug concentration over the range of 50 ng ml(-1) to 25.6 μg ml(-1). The achieved limit of detection and limit of quantitation were 3.99 and 13.3 ng ml(-1) by SWCAdSV and 7.98 and 26.6 ng ml(-1) by DPCAdSV, respectively. The procedure was applied to assay the drug in tablets. Applicability was also tested in urine samples. Peak current was linear with the drug concentration in the range of 1 to 60 μg ml(-1) of the urine, and minimum detectability was found to be 12.6 ng ml(-1) by SWCAdSV and 58.4 ng ml(-1) by DPCAdSV. PMID:20678464

An implantable, micromachined microprobe with a microsensor array for combined monitoring of the neurotransmitters, glutamate (Glut) and dopamine (DA), by constant potential amperometry has been created and characterized. Microprobe studies in vitro revealed Glut and DA microsensor sensitivities of 126±5 nA·μM(-1)·cm(-2) and 3250±50 nA·μM(-1)·cm(-2), respectively, with corresponding detection limits of 2.1±0.2 μM and 62±8 nM, both at comparable ~1 sec response times. No diffusional interaction of H(2)O(2) among arrayed microelectrodes was observed. Also, no responses from the electroactive interferents, ascorbic acid (AA), uric acid (UA), DOPA (a DA catabolite) or DOPAC (a DA precursor), over their respective physiological concentration ranges, were detected. The dual sensing microbe attributes of size, detection limit, sensitivity, response time and selectivity make it attractive for combined sensing of Glut and DA in vivo. PMID:23139647

A fuel cell has the potential to become an important source of electric power. However, measuring the temperature inside the fuel cell is difficult. Hence, in this investigation, an array of microsensors is set up inside the fuel cell to measure the temperature distribution. The substrate of a bipolar plate in the fuel cell is stainless steel (SS-316) and an electroforming technique is implemented to fabricate channels in the stainless steel substrate. Then micro-electro-mechanical system (MEMS) technologies are employed to fabricate a platinum temperature sensor on the rib of a channel in the stainless steel substrate. In this experiment, the temperature of microsensor is measured to range from 31 to 80 °C and its resistance ranges from 0.593 to 0.649 Ω. Experimental results demonstrate that temperature is almost linearly related to resistance and that accuracy and sensitivity are 0.5 °C and 1.93× 10-3/°C, respectively. The performance curves of a single fuel cell operating at 34 °C and H2/O2 gas flow rates of 50/50 ml/min are determined. The maximum power density is 170 mW/cm2 and the current density is 513 mA/cm2.

Carbon dioxide (CO2) is one of the major indicators of fire and therefore its measurement is very important for low-false-alarm fire detection and emissions monitoring. However, only a limited number of CO2 sensing materials exist due to the high chemical stability of CO2. In this work, a novel CO2 microsensor based on nanocrystalline tin oxide (SnO2) doped with copper oxide (CuO) has been successfully demonstrated. The CuO-SnO2 based CO2 microsensors are fabricated by means of microelectromechanical systems (MEMS) technology and sol-gel nanomaterial-synthesis processes. At a doping level of CuO: SnO2 = 1:8 (molar ratio), the resistance of the sensor has a linear response to CO2 concentrations for the range of 1 to 4 percent CO2 in air at 450 C. This approach has demonstrated the use of SnO2, typically used for the detection of reducing gases, in the detection of an oxidizing gas.

In this study, an application of a voltammetric electronic tongue for discrimination and prediction of different varieties of rice was investigated. Different pretreatment methods were selected, which were subsequently used for the discrimination of different varieties of rice and prediction of unknown rice samples. To this aim, a voltammetric array of sensors based on metallic electrodes was used as the sensing part. The different samples were analyzed by cyclic voltammetry with two sample-pretreatment methods. Discriminant Factorial Analysis was used to visualize the different categories of rice samples; however, radial basis function (RBF) artificial neural network with leave-one-out cross-validation method was employed for prediction modeling. The collected signal data were first compressed employing fast Fourier transform (FFT) and then significant features were extracted from the voltammetric signals. The experimental results indicated that the sample solutions obtained by the non-crushed pretreatment method could efficiently meet the effect of discrimination and recognition. The satisfactory prediction results of voltammetric electronic tongue based on RBF artificial neural network were obtained with less than five-fold dilution of the sample solution. The main objective of this study was to develop primary research on the application of an electronic tongue system for the discrimination and prediction of solid foods and provide an objective assessment tool for the food industry. PMID:26205274

In this work, a dual-nanomaterial based electrode was established for selective and sensitive detection of trace Fe(II) in the presence of complexing agent (2,2'-bipyridyl). Titanium carbide nanoparticles (TiCNPs) were used as the growth-template for the formation of three-dimensional platinum nanoflowers (PtNFs) due to their unique cubic structures. Nafion was employed as the conducting matrix to help TiCNPs better attached onto the surface of the electrode and slow down the crystal rate of PtNFs during electrodeposition, which resulted in flower structure and more active surface of PtNFs. Taking advantage of synergistic effects of TiCNPs and Nafion as well as the catalytic amplifying effect of PtNFs, the excellent anodic signal responses for the voltammetric stripping determination of Fe(II) were obtained. The linear range of Fe(II) on this dual-nanomaterial based electrode was from 1nmolL(-1) to 6μmolL(-1) with the lowest detectable concentration of 0.1nmolL(-1) and a detection limit of 0.03nmolL(-1). Additionally, the effect of several experimental parameters, such as concentration and pH value of buffer solution, concentration of modifier and ligand, deposition potential and time of electrochemical determination, and scan rate were studied for analytical applications. The fabricated sensor had been successfully applied for the sensitive determination of trace Fe(II) in coastal waters. PMID:27154657

A detailed study of iron (III)-citrate speciation in aqueous solution (θ=25°C, I(c)=0.7 mol L(-1)) was carried out by voltammetric and UV-vis spectrophotometric measurements and the obtained data were used for reconciled characterization of iron (III)-citrate complexes. Four different redox processes were registered in the voltammograms: at 0.1 V (pH=5.5) which corresponded to the reduction of iron(III)-monocitrate species (Fe:cit=1:1), at about -0.1 V (pH=5.5) that was related to the reduction of FeL(2)(5-), FeL(2)H(4-) and FeL(2)H(2)(3-) complexes, at -0.28 V (pH=5.5) which corresponded to the reduction of polynuclear iron(III)-citrate complex(es), and at -0.4V (pH=7.5) which was probably a consequence of Fe(cit)(2)(OH)(x) species reduction. Reversible redox process at -0.1 V allowed for the determination of iron(III)-citrate species and their stability constants by analyzing E(p) vs. pH and E(p) vs. [L(4-)] dependence. The UV-vis spectra recorded at varied pH revealed four different spectrally active species: FeLH (logβ=25.69), FeL(2)H(2)(3-) (log β=48.06), FeL(2)H(4-) (log β=44.60), and FeL(2)(5-) (log β=38.85). The stability constants obtained by spectrophotometry were in agreement with those determined electrochemically. The UV-vis spectra recorded at various citrate concentrations (pH=2.0) supported the results of spectrophotometric-potentiometric titration. PMID:22938610

Thin films of the bis[2,3,9,10,16,17,23,24-octachlorophthalocyaninate] lutetium(III) complex (LuPc2Cl32) have been prepared by the Langmuir-Blodgett and the Langmuir-Schaefer (LS) techniques. The influence of the chlorine substituents in the structure of the films and in their spectroscopic, electrochemical and sensing properties has been evaluated. The π-A isotherms exhibit a monolayer stability greater than the observed in the unsubstituted analogue (LuPc2), being easily transferred to solid substrates, also in contrast to LuPc2. The LB and LS films present a linear growth forming stratified layers, monitored by UV-VIS absorption spectroscopy. The latter also revealed the presence of LuPc2Cl32 in the form of monomers and aggregates in both films. The FTIR data showed that the LuPc2Cl32 molecules present a non-preferential arrangement in both films. Monolayers of LB and LS were deposited onto 6 nm Ag island films to record surface-enhanced resonance Raman scattering (SERRS), leading to enhancement factors close to 2 x 10(3). Finally, LB and LS films deposited onto ITO glass have been successfully used as voltammetric sensors for the detection of catechol. The improved electroactivity of the LB and LS films has been confirmed by the reduction of the overpotential of the oxidation of catechol. The enhancement of the electrocatalytic effect observed in LB and LS films is the result of the nanostructured arrangement of the surface which increases the number of active sites. The sensors show a limit of detection in the range of 10(-5) mol/L. PMID:25924327

A humidity microsensor integrated with a readout circuit on-a-chip fabricated using the commercial 0.18 μm CMOS (complementary metal oxide semiconductor) process was presented. The integrated sensor chip consists of a humidity sensor and a readout circuit. The humidity sensor is composed of a sensitive film and interdigitated electrodes. The sensitive film is titanium dioxide prepared by the sol-gel method. The titanium dioxide is coated on the interdigitated electrodes. The humidity sensor requires a post-process to remove the sacrificial layer and to coat the titanium dioxide. The resistance of the sensor changes as the sensitive film absorbs or desorbs vapor. The readout circuit is employed to convert the resistance variation of the sensor into the output voltage. The experimental results show that the integrated humidity sensor has a sensitivity of 4.5 mV/RH% (relative humidity) at room temperature. PMID:24594612

The accurate and rapid measurement of physiological O2 transport is vital for understanding spatially and temporally dynamic metabolism and stress signalling in plant cells and tissues. Single channel luminescent O2- quenched optrodes have been available for use in laboratory and field experiments since the early 2000's. However, to collect the large datasets needed to understand O2 transport in complex systems, many experiments require a multiple channel O2 sensor system. This research reports the development of a multiplexing fiber optic O2 microsensor system designed to conduct high temporal resolution experiments for field studies of plant physiology. The 10 channel system was demonstrated for measuring O2 concentration in developing soybean seeds (Glycine max L. Merr.) within a climate controlled greenhouse.

Development of PCB-integrateable microsensors for monitoring chemical species is a goal in areas such as lab-on-a-chip analytical devices, diagnostics medicine and electronics for hand-held instruments where the device size is a major issue. Cellular phones have pervaded the world inhabitants and their usefulness has dramatically increased with the introduction of smartphones due to a combination of amazing processing power in a confined space, geolocalization and manifold telecommunication features. Therefore, a number of physical and chemical sensors that add value to the terminal for health monitoring, personal safety (at home, at work) and, eventually, national security have started to be developed, capitalizing also on the huge number of circulating cell phones. The chemical sensor-enabled "super" smartphone provides a unique (bio)sensing platform for monitoring airborne or waterborne hazardous chemicals or microorganisms for both single user and crowdsourcing security applications. Some of the latest ones are illustrated by a few examples. Moreover, we have recently achieved for the first time (covalent) functionalization of p- and n-GaN semiconductor surfaces with tuneable luminescent indicator dyes of the Ru-polypyridyl family, as a key step in the development of innovative microsensors for smartphone applications. Chemical "sensoring" of GaN-based blue LED chips with those indicators has also been achieved by plasma treatment of their surface, and the micrometer-sized devices have been tested to monitor O2 in the gas phase to show their full functionality. Novel strategies to enhance the sensor sensitivity such as changing the length and nature of the siloxane buffer layer are discussed in this paper.

The physical demands of rugby league, rugby union, and American football are significantly increased through the large number of collisions players are required to perform during match play. Because of the labor-intensive nature of coding collisions from video recordings, manufacturers of wearable microsensor (e.g., global positioning system [GPS]) units have refined the technology to automatically detect collisions, with several sport scientists attempting to use these microsensors to quantify the physical demands of collision sports. However, a question remains over the validity of these microtechnology units to quantify the contact demands of collision sports. Indeed, recent evidence has shown significant differences in the number of "impacts" recorded by microtechnology units (GPSports) and the actual number of collisions coded from video. However, a separate study investigated the validity of a different microtechnology unit (minimaxX; Catapult Sports) that included GPS and triaxial accelerometers, and also a gyroscope and magnetometer, to quantify collisions. Collisions detected by the minimaxX unit were compared with video-based coding of the actual events. No significant differences were detected in the number of mild, moderate, and heavy collisions detected via the minimaxX units and those coded from video recordings of the actual event. Furthermore, a strong correlation (r = 0.96, p < 0.01) was observed between collisions recorded via the minimaxX units and those coded from video recordings of the event. These findings demonstrate that only one commercially available and wearable microtechnology unit (minimaxX) can be considered capable of offering a valid method of quantifying the contact loads that typically occur in collision sports. Until such validation research is completed, sport scientists should be circumspect of the ability of other units to perform similar functions. PMID:23090320

An article of manufacture is provided including a substrate having an oxide surface layer and a selective thin film of a cyclodextrin derivative chemically bound upon said substrate, said film is adapted for the inclusion of a selected organic compound therewith. Such an article can be either a chemical sensor capable of detecting a resultant mass change from inclusion of the selected organic compound or a chemical separator capable of reversibly selectively separating a selected organic compound.

This study investigates the fabrication and characterization of an acetone microsensor with a ring oscillator circuit using the commercial 0.18 μm complementary metal oxide semiconductor (CMOS) process. The acetone microsensor contains a sensitive material, interdigitated electrodes and a polysilicon heater. The sensitive material is α-Fe2O3 synthesized by the hydrothermal method. The sensor requires a post-process to remove the sacrificial oxide layer between the interdigitated electrodes and to coat the α-Fe2O3 on the electrodes. When the sensitive material adsorbs acetone vapor, the sensor produces a change in capacitance. The ring oscillator circuit converts the capacitance of the sensor into the oscillation frequency output. The experimental results show that the output frequency of the acetone sensor changes from 128 to 100 MHz as the acetone concentration increases 1 to 70 ppm. PMID:25036331

The voltammetric behavior of a carbon paste electrode modified with Co(II)-exchanged zeolite A (Co(II)-A/ZMCPE) for determination of acetaminophen was studied. The proposed electrode showed a diffusion controlled reaction with the electron transfer rate constant (Ks) of 0.44s(-1) and charge transfer coefficient of 0.73 in the absence of acetaminophen. A linear voltammetric response was obtained in the range of 0.1 to 190μmolL(-1) of acetaminophen [r(2)=0.9979, r=0.9989 (n=10)] with a detection limit of 0.04μmolL(-1). The method was successfully applied to the analysis of acetaminophen in some drugs. PMID:25686976

A recently published method for quantifying refractory organic matter (often referred to as humic substances) in freshwaters was applied to a wide range of International Humic Substance Society (IHSS) humic compounds in order to (i) gain a better understanding of the mechanism of the voltammetric response which is the basis of the analytical method and (ii) provide guidance on choosing the optimal standard to be used. At the same time, the sensitivity of the technique has been increased by switching from the pulse mode initially proposed to the square-wave mode. The results obtained show that (i) differences in adsorption onto the electrode rather than differences in complexation strength are responsible for the differences in the intensity of the signal obtained for the different humic compounds, (ii) carboxylate, N- and S-containing groups do not play a role in the voltammetric signal. PMID:18791870

The electrochemical oxidation of salicylic acid (SA) has been studied on a glassy carbon electrode using cyclic voltammetry and differential pulse voltammetric (DPV) method. SA gives a single irreversible oxidation wave over the wide pH range studied. The irreversibility of the electrode process was verified by different criteria. The mechanism of oxidation is discussed. Using differential pulse voltammetry, SA yielded a well-defined voltammetric response in Britton-Robinson buffer solution, pH 2.37 at 1.088V (versus Ag/AgCl). The method was linear over the SA concentration range: 1-60mugml(-1). The method was successfully applied for the analysis of SA as a hydrolysis product, in solid pharmaceutical formulations containing acetylsalicylic acid (ASA). PMID:18969288

The voltammetric response of Au and Pt microdisk electrodes (6.4, 12.5, and 25 {micro}m) in concentrated solutions of organic redox species (nitrobenzene, acetophenone, and benzophenone) has been measured as a function of the orientation and magnitude of an externally applied magnetic field (0--1 Tesla). A magnetic field effect on voltammetric currents is observed for redox concentrations greater than ca. 0.01 M, and is a strong function of the orientation of the field. Large enhancements (+100%) or diminishments ({minus}15%) of limiting currents can be induced by application of the magnetic field. The observed phenomena are discussed in terms of magnetic field-induced transport of electrogenerated products.

We describe an ultrasensitive voltammetric detection of trace heavy metal ions using nanoelectrode arrays (NEAs) that are based on low-site density carbon nanotubes (CNTs). The NEAs were prepared by sealing the side-walls of CNTs with an epoxy passive layer that reduces the current leakage and eliminates the electrode capacitance, leading to a low background current. This provides a high signal-to-noise ratio. The CNTs-NEAs coated with a bismuth film were used successfully for voltammetric detection of trace cadmium and lead (II) at the sub-ppb level. The detection limit of 0.04 {micro}g/L was obtained under optimum experimental conditions. The attractive behavior of the new carbon NEA sensing platform holds great promise for onsite environmental monitoring and biomonitoring of toxic metals.

A classification method of discriminate rice from different varieties with voltammetric electronic tongue based on square wave voltammetry is investigated. The rice samples are crushed and mixed with distilled water to get the rice solution, and the solution should be stirred and filtered before the experiment. In order to obtain the electrochemical response signals of the rice samples and extract the characteristic value of the singles, the electronic tongue which works respectively with titanium (Ti) electrode and tungsten electrode (W) to test the sample solution under square wave voltammetry. The Principal Component Analysis (PCA) and Clustering Analysis (CA) are adopted to classify and recognize the rice samples. Experimental results show that good classification and recognition results are got in this paper when using Principal Component Analysis and Cluster Analysis to analyze the response signals which are obtained by voltammetric electronic tongue worked with Ti electrode and W electrode under square wave potential.

Voltammetric studies on the simple ion transfer (IT) behaviors of an important water-soluble B-vitamin, folic acid (FA), at the liquid-liquid (L-L) interface were firstly performed and then applied as a novel detection method for FA under physiological conditions. Meso-water-1,6-dichlorohexane (W-DCH) and meso-water-organogel interface arrays were built by using a hybrid mesoporous silica membrane (HMSM) with a unique structure of pores-in-pores and employed as the new platforms for the IT voltammetric study. In view of the unique structure of the HMSM, the impact of the ionic surfactant cetyltrimethylammonium bromide (CTAB), self-assembled within the silica nanochannels of the HMSM, was investigated. In particular, its effect on the IT voltammetric behavior and detection of FA at meso-L-L interface arrays was systematically examined by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and differential pulse stripping voltammetry (DPSV). It was found that all the voltammetric responses of CV, DPV, and DPSV and the corresponding detection limit of FA at such meso-L-L interface arrays are closely related to the CTAB in the HMSM. Significantly, the calculated detection limit of FA could be improved to 80 nM after the combination of the DPSV technique with the additional preconcentration of FA in the silica-CTAB nanochannels, achieved through an anion-exchange process between FA(-) and the bromide of CTAB in HMSM. This provides a new and attractive strategy for the detection of those biological anions. PMID:25730302

Principal component regression has been used in the past to separate current contributions from different neuromodulators measured with in vivo fast-scan cyclic voltammetry. Traditionally, a percent cumulative variance approach has been used to determine the rank of the training set voltammetric matrix during model development, however this approach suffers from several disadvantages including the use of arbitrary percentages and the requirement of extreme precision of training sets. Here we propose that Malinowski’s F-test, a method based on a statistical analysis of the variance contained within the training set, can be used to improve factor selection for the analysis of in vivo fast-scan cyclic voltammetric data. These two methods of rank estimation were compared at all steps in the calibration protocol including the number of principal components retained, overall noise levels, model validation as determined using a residual analysis procedure, and predicted concentration information. By analyzing 119 training sets from two different laboratories amassed over several years, we were able to gain insight into the heterogeneity of in vivo fast-scan cyclic voltammetric data and study how differences in factor selection propagate throughout the entire principal component regression analysis procedure. Visualizing cyclic voltammetric representations of the data contained in the retained and discarded principal components showed that using Malinowski’s F-test for rank estimation of in vivo training sets allowed for noise to be more accurately removed. Malinowski’s F-test also improved the robustness of our criterion for judging multivariate model validity, even though signal-to-noise ratios of the data varied. In addition, pH change was the majority noise carrier of in vivo training sets while dopamine prediction was more sensitive to noise. PMID:20527815

This Final Report describes efforts and results for a 3-year DoE/OST-EMSP project centered at NIST. The multidisciplinary project investigated scientific and technical concepts critical for developing tunable, MEMS-based, gas and vapor microsensors that could be applied for monitoring the types of multiple analytes (and differing backgrounds) encountered at DoE waste sites. Micromachined ''microhotplate'' arrays were used as platforms for fabricating conductometric sensor prototypes, and as microscale research tools. Efficient microarray techniques were developed for locally depositing and then performance evaluating thin oxide films, in order to correlate gas sensing characteristics with properties including composition, microstructure, thickness and surface modification. This approach produced temperature-dependent databases on the sensitivities of sensing materials to varied analytes (in air) which enable application-specific tuning of microsensor arrays. Mechanistic studies on adsorb ate transient phenomena were conducted to better understand the ways in which rapid temperature programming schedules can be used to produce unique response signatures and increase information density in microsensor signals. Chemometric and neural network analyses were also employed in our studies for recognition and quantification of target analytes.

Herein we report the first serum insulin voltammetric immunosensor for diagnosis of type 1 and type 2 diabetic disorders. The sensor is composed of multiwalled carbon nanotube-pyrenebutyric acid frameworks on edge plane pyrolytic graphite electrodes (PGE/MWNT/Py) to which an anti-insulin antibody was covalently attached. The detection of picomolar levels of serum insulin binding to the surface antibody was achieved by monitoring the decrease in voltammetric current signals of a redox probe taken in the electrolyte solution. This method offered a detection limit of 15 pM for free insulin present in serum. This detection limit was further lowered to 5 pM by designing serum insulin conjugates with poly(acrylic acid)-functionalized magnetite nanoparticles (100 nm hydrodynamic diameter) and detecting the binding of MNP-serum insulin conjugate to the surface insulin-antibody on PGE/MWNT/Py electrodes. When tested on real patient serum samples, the sensor accurately measured insulin levels. To our knowledge, this is the first report of a voltammetric immunosensor capable of both diagnosing and distinguishing the type of diabetes based on serum insulin levels in diabetic patients. PMID:25675332

Background Support vector regression (SVR) and Gaussian process regression (GPR) were used for the analysis of electroanalytical experimental data to estimate diffusion coefficients. Results For simulated cyclic voltammograms based on the EC, Eqr, and EqrC mechanisms these regression algorithms in combination with nonlinear kernel/covariance functions yielded diffusion coefficients with higher accuracy as compared to the standard approach of calculating diffusion coefficients relying on the Nicholson-Shain equation. The level of accuracy achieved by SVR and GPR is virtually independent of the rate constants governing the respective reaction steps. Further, the reduction of high-dimensional voltammetric signals by manual selection of typical voltammetric peak features decreased the performance of both regression algorithms compared to a reduction by downsampling or principal component analysis. After training on simulated data sets, diffusion coefficients were estimated by the regression algorithms for experimental data comprising voltammetric signals for three organometallic complexes. Conclusions Estimated diffusion coefficients closely matched the values determined by the parameter fitting method, but reduced the required computational time considerably for one of the reaction mechanisms. The automated processing of voltammograms according to the regression algorithms yields better results than the conventional analysis of peak-related data. PMID:24987463

Histamine and serotonin are neuromodulators which facilitate numerous, diverse neurological functions. Being co-localized in many brain regions, these two neurotransmitters are thought to modulate one another's chemistry and are often implicated in the etiology of disease. Thus, it is desirable to interpret the in vivo chemistry underlying neurotransmission of these two molecules to better define their roles in health and disease. In this work, we describe a voltammetric approach to monitoring serotonin and histamine simultaneously in real time. Via electrical stimulation of the axonal bundles in the medial forebrain bundle, histamine release was evoked in the mouse premammillary nucleus. We found that histamine release was accompanied by a rapid, potent inhibition of serotonin in a concentration-dependent manner. We developed mathematical models to capture the experimental time courses of histamine and serotonin, which necessitated incorporation of an inhibitory receptor on serotonin neurons. We employed pharmacological experiments to verify that this serotonin inhibition was mediated by H3 receptors. Our novel approach provides fundamental mechanistic insights that can be used to examine the full extent of interconnectivity between histamine and serotonin in the brain. Histamine and serotonin are co-implicated in many of the brain's functions. In this paper, we develop a novel voltammetric method for simultaneous real-time monitoring of histamine and serotonin in the mouse premammillary nucleus. Electrical stimulation of the medial forebrain bundle evokes histamine and inhibits serotonin release. We show voltammetrically, mathematically, and pharmacologically that this serotonin inhibition is H3 receptor mediated. PMID:27167463

In previous studies a novel amphiphilic co-polymer was developed for use in lithium-ion batteries. In order to evaluate the electrochemical stability of that electrolyte and compare it with others, a voltammetric method was applied on a set of electrolytes with different salts, solvents and polymers. However, initially the voltammetric methodology was studied. Platinum was found to be the most suited electrode material, experiencing no significant interfering reactions and a proper diffusion-controlled kinetic behaviour when sweep rate was varied. Furthermore, the influence on the voltammograms of adding water traces to the electrolytes was studied. It could be established that the oxidation peak around 3.8 V versus Li was related to water reactions. It was concluded that quantitative voltage values of the stability limits were difficult to assess using voltammetry. On the other hand, the method seemed well suited for comparison of electrolytes and to investigate the influences of electrolyte components on the stability. The voltammetric results varied little between the different electrolytes evaluated and the anodic and cathodic limits, as defined here, were in the range of 1 and 4.5 V vs. Li, respectively. Although the novel polymer did not affect the stability limit significantly it seemed to promote the breakdown reaction rate in all electrolytes tested. Furthermore, the use of LiTFSI salt reduced the stability window.

This unit describes the preparation and applications of porphyrinic sensors for quantitative measurement of nitric oxide (NO) in single cells and in tissues. The determination of NO is based on the electrochemical oxidation of NO on a carbon fiber electrode covered with a thin layer of a conducting polymeric metalloporphyrin catalyst, overlaid with another thin film of Nafion, a cation exchange material. The electric current generated during NO oxidation on the surface of the polymeric porphyrin is linearly proportional to the concentration of NO, so this current is used as an analytical signal which can be measured in either the amperometric or the voltammetric mode. Both methods provide a quantitative signal. This unit describes the electrochemical setup for measurement of NO in single cells and tissue. Support protocols describe porphyrin synthesis, sensor preparation, and sensor calibration. PMID:18428525

Waste characterization is probably the most costly part of radioactive waste management. An important part of this characterization is the measurements of headspace gas in waste containers in order to demonstrate the compliance with Resource Conservation and Recovery Act (RCRA) or transportation requirements. The traditional chemical analysis methods, which include all steps of gas sampling, sample shipment and laboratory analysis, are expensive and time-consuming as well as increasing worker's exposure to hazardous environments. Therefore, an alternative technique that can provide quick, in-situ, and real-time detections of headspace gas compositions is highly desirable. This report summarizes the results obtained from a Laboratory Directed Research & Development (LDRD) project entitled 'Potential Application of Microsensor Technology in Radioactive Waste Management with Emphasis on Headspace Gas Detection'. The objective of this project is to bridge the technical gap between the current status of microsensor development and the intended applications of these sensors in nuclear waste management. The major results are summarized below: {sm_bullet} A literature review was conducted on the regulatory requirements for headspace gas sampling/analysis in waste characterization and monitoring. The most relevant gaseous species and the related physiochemical environments were identified. It was found that preconcentrators might be needed in order for chemiresistor sensors to meet desired detection {sm_bullet} A long-term stability test was conducted for a polymer-based chemresistor sensor array. Significant drifts were observed over the time duration of one month. Such drifts should be taken into account for long-term in-situ monitoring. {sm_bullet} Several techniques were explored to improve the performance of sensor polymers. It has been demonstrated that freeze deposition of black carbon (CB)-polymer composite can effectively eliminate the so-called 'coffee ring

An ambient temperature oxygen microsensor, based on a Nafion polymer electrolyte, has been developed and was microfabricated using thin-film technologies. A challenge in the operation of Nafion-based sensor systems is that the conductivity of Nafion film depends on the humidity in the film. Nafion film loses conductivity when the moisture content in the film is too low, which can affect sensor operation. The advancement here is the identification of a method to retain the operation of the Nafion films in lower humidity environments. Certain salts can hold water molecules in the Nafion film structure at room temperature. By mixing salts with the Nafion solution, water molecules can be homogeneously distributed in the Nafion film increasing the film s hydration to prevent Nafion film from being dried out in low-humidity environment. The presence of organics provides extra sites in the Nafion film to promote proton (H+) mobility and thus improving Nafion film conductivity and sensor performance. The fabrication of ambient temperature oxygen microsensors includes depositing basic electrodes using noble metals, and metal oxides layer on one of the electrode as a reference electrode. The use of noble metals for electrodes is due to their strong catalytic properties for oxygen reduction. A conducting polymer Nafion, doped with water-retaining components and extra sites facilitating proton movement, was used as the electrolyte material, making the design adequate for low humidity environment applications. The Nafion solution was coated on the electrodes and air-dried. The sensor operates at room temperature in potentiometric mode, which measures voltage differences between working and reference electrodes in different gases. Repeat able responses to 21-percent oxygen in nitrogen were achieved using nitrogen as a baseline gas. Detection of oxygen from 7 to 21 percent has also been demonstrated. The room-temperature oxygen micro sensor developed has extremely low power

Anthropogenic elemental mercury (Hg0) emission is a serious worldwide environmental problem due to the extreme toxicity of the heavy metal to humans, plants and wildlife. Development of an accurate and cheap microsensor based online monitoring system which can be integrated as part of Hg0 removal and control processes in industry is still a major challenge. Here, we demonstrate that forming Au nanospike structures directly onto the electrodes of a quartz crystal microbalance (QCM) using a novel electrochemical route results in a self-regenerating, highly robust, stable, sensitive and selective Hg0 vapor sensor. The data from a 127 day continuous test performed in the presence of volatile organic compounds and high humidity levels, showed that the sensor with an electrodeposted sensitive layer had 260% higher response magnitude, 3.4 times lower detection limit (~22 μg/m3 or ~2.46 ppbv) and higher accuracy (98% Vs 35%) over a Au control based QCM (unmodified) when exposed to a Hg0 vapor concentration of 10.55 mg/m3 at 101°C. Statistical analysis of the long term data showed that the nano-engineered Hg0 sorption sites on the developed Au nanospikes sensitive layer play a critical role in the enhanced sensitivity and selectivity of the developed sensor towards Hg0 vapor.

Stochastic microsensors based on diamond paste and three types of electroactive materials (maltodextrin (MD), α-cyclodextrin (α-CD) and 5,10,15,20-tetraphenyl-21H,23H porphyrin (P)) were developed for the assay of estradiol (E2), testosterone (T2) and dihydrotestosterone (DHT) in children's saliva. The main advantage of utilization of such tools is the possibility to identify and quantify all three hormones within minutes in small volumes of childen's saliva. The limits of quantification obtained for DHT, T2, and E2 (1 fmol/L for DHT, 1 pmol/L for T2, and 66 fmol/L for E2) determined using the proposed tools allows the utilization of these new methods with high reliability for the screening of saliva samples from children. This new method proposed for the assay of the three hormones overcomes the limitations (regarding limits of determination) of ELISA method which is the standard method used in clinical laboratories for the assay of DHT, T2, and E2 in saliva samples. The main feature of its utilization for children's saliva is to identify earlier problems related to early puberty and obesity. PMID:24993181

A sensitive thermal microsensor based on a pn junction diode for heat measurements of biological single cells is developed and evaluated. Using a fabricated device, we demonstrated the heat measurement of a single brown fat cell. The principle of the sensor relies on the temperature dependence of the pn junction diode resistance. This method has a capability of the highly thermal sensitivity by downsizing and the advantage of a simple experimental setup using electrical circuits without any special equipment. To achieve highly sensitive heat measurement of single cells, downsizing of the sensor is necessary to reduce the heat capacity of the sensor itself. The sensor with the pn junction diode can be downsized by microfabrication. A bridge beam structure with the pn junction diode as a thermal sensor is placed in vacuum using a microfludic chip to decrease the heat loss to the surroundings. A temperature coefficient of resistance of 1.4%/K was achieved. The temperature and thermal resolutions of the fabricated device are 1.1 mK and 73.6 nW, respectively. The heat measurements of norepinephrine stimulated and nonstimulated single brown fat cells were demonstrated, and different behaviors in heat generation were observed.

The microzonation of O2 respiration, H2S oxidation, and SO42- reduction in aerobic trickling-filter biofilms was studied by measuring concentration profiles at high spatial resolution (25 to 100 μm) with microsensors for O2, S2-, and pH. Specific reaction rates were calculated from measured concentration profiles by using a simple one-dimensional diffusion reaction model. The importance of electron acceptor and electron donor availability for the microzonation of respiratory processes and their reaction rates was investigated. Oxygen respiration was found in the upper 0.2 to 0.4 mm of the biofilm, whereas sulfate reduction occurred in deeper, anoxic parts of the biofilm. Sulfate reduction accounted for up to 50% of the total mineralization of organic carbon in the biofilms. All H2S produced from sulfate reduction was reoxidized by O2 in a narrow reaction zone, and no H2S escaped to the overlying water. Turnover times of H2S and O2 in the reaction zone were only a few seconds owing to rapid bacterial H2S oxidation. Anaerobic H2S oxidation with NO3- could be induced by addition of nitrate to the medium. Total sulfate reduction rates increased when the availability of SO42- or organic substrate increased as a result of deepening of the sulfate reduction zone or an increase in the sulfate reduction intensity, respectively. PMID:16348687

In this study we present the real-time monitoring of three key brain neurochemical species in conscious rats using implantable amperometric electrodes interfaced to a biotelemetric device. The new system, derived from a previous design, was coupled with carbon-based microsensors and a platinum-based biosensor for the detection of ascorbic acid (AA), O2 and glucose in the striatum of untethered, freely-moving rats. The miniaturized device consisted of a single-supply sensor driver, a current-to-voltage converter, a microcontroller and a miniaturized data transmitter. The redox currents were digitized to digital values by means of an analog-to-digital converter integrated in a peripheral interface controller (PIC), and sent to a personal computer by means of a miniaturized AM transmitter. The electronics were calibrated and tested in vitro under different experimental conditions and exhibited high stability, low power consumption and good linear response in the nanoampere current range. The in-vivo results confirmed previously published observations on striatal AA, oxygen and glucose dynamics recorded in tethered rats. This approach, based on simple and inexpensive components, could be used as a rapid and reliable model for studying the effects of different drugs on brain neurochemical systems. PMID:22574029

In micro-sensor motion capture systems, the estimation of the body displacement in the global coordinate system remains a challenge due to lack of external references. This paper proposes a self-contained displacement estimation method based on a human biomechanical model to track the position of walking subjects in the global coordinate system without any additional supporting infrastructures. The proposed approach makes use of the biomechanics of the lower body segments and the assumption that during walking there is always at least one foot in contact with the ground. The ground contact joint is detected based on walking gait characteristics and used as the external references of the human body. The relative positions of the other joints are obtained from hierarchical transformations based on the biomechanical model. Anatomical constraints are proposed to apply to some specific joints of the lower body to further improve the accuracy of the algorithm. Performance of the proposed algorithm is compared with an optical motion capture system. The method is also demonstrated in outdoor and indoor long distance walking scenarios. The experimental results demonstrate clearly that the biomechanical model improves the displacement accuracy within the proposed framework.

Low cost access to space is a primary goal for both NASA and the U.S. aerospace industry. Integrated subsystem health diagnostics is an area where major improvements have been identified for potential implementation into the design of new reusable launch vehicles (RLVS) in order to reduce life cycle costs, increase safety margins and improve mission reliability. A number of efforts are underway to use existing and emerging technologies to establish new methods for vehicle health monitoring on operational vehicles as well as X-vehicles. This paper summarizes a joint effort between several NASA centers and industry partners to develop rapid wireless diagnostic tools for failure management and long-term TPS performance monitoring of thermal protection systems (TPS) on future RLVS. An embedded wireless microsensor suite is being designed to allow rapid subsurface TPS health monitoring and damage assessment. This sensor suite will consist of both passive overlimit sensors and sensors for continuous parameter monitoring in flight. The on-board diagnostic system can be used to radio in maintenance requirements before landing and the data could also be used to assist in design validation for X-vehicles. For a 3rd generation vehicle, wireless diagnostics should be at a stage of technical development that will allow use for intelligent feedback systems for guidance and navigation control applications and can also serve as feedback for TPS that can intelligently adapt to its environment.

Stochastic microsensors based on diamond paste and three types of electroactive materials (maltodextrin (MD), α-cyclodextrin (α-CD) and 5,10,15,20-tetraphenyl-21H,23H porphyrin (P)) were developed for the assay of estradiol (E2), testosterone (T2) and dihydrotestosterone (DHT) in children's saliva. The main advantage of utilization of such tools is the possibility to identify and quantify all three hormones within minutes in small volumes of childen's saliva. The limits of quantification obtained for DHT, T2, and E2 (1 fmol/L for DHT, 1 pmol/L for T2, and 66 fmol/L for E2) determined using the proposed tools allows the utilization of these new methods with high reliability for the screening of saliva samples from children. This new method proposed for the assay of the three hormones overcomes the limitations (regarding limits of determination) of ELISA method which is the standard method used in clinical laboratories for the assay of DHT, T2, and E2 in saliva samples. The main feature of its utilization for children's saliva is to identify earlier problems related to early puberty and obesity.

The effectiveness of a wearable microsensor device (MinimaxX(TM) S4, Catapult Innovations, Melbourne, VIC, Australia) to automatically detect tackles and impact events in elite Australian football (AF) was assessed during four matches. Video observation was used as the criterion measure. A total of 352 tackles were observed, with 78% correctly detected as tackles by the manufacturer's software. Tackles against (i.e. tackled by an opponent) were more accurately detected than tackles made (90% v 66%). Of the 77 tackles that were not detected at all, the majority (74%) were categorised as low-intensity. In contrast, a total of 1510 "tackle" events were detected, with only 18% of these verified as tackles. A further 57% were from contested ball situations involving player contact. The remaining 25% were in general play where no contact was evident; these were significantly lower in peak Player Load™ than those involving player contact (P < 0.01). The tackle detection algorithm, developed primarily for rugby, was not suitable for tackle detection in AF. The underlying sensor data may have the potential to detect a range of events within contact sports such as AF, yet to do so is a complex task and requires sophisticated sport and event-specific algorithms. PMID:24499311

Anthropogenic elemental mercury (Hg0) emission is a serious worldwide environmental problem due to the extreme toxicity of the heavy metal to humans, plants and wildlife. Development of an accurate and cheap microsensor based online monitoring system which can be integrated as part of Hg0 removal and control processes in industry is still a major challenge. Here, we demonstrate that forming Au nanospike structures directly onto the electrodes of a quartz crystal microbalance (QCM) using a novel electrochemical route results in a self-regenerating, highly robust, stable, sensitive and selective Hg0 vapor sensor. The data from a 127 day continuous test performed in the presence of volatile organic compounds and high humidity levels, showed that the sensor with an electrodeposted sensitive layer had 260% higher response magnitude, 3.4 times lower detection limit (~22 μg/m3 or ~2.46 ppbv) and higher accuracy (98% Vs 35%) over a Au control based QCM (unmodified) when exposed to a Hg0 vapor concentration of 10.55 mg/m3 at 101°C. Statistical analysis of the long term data showed that the nano-engineered Hg0 sorption sites on the developed Au nanospikes sensitive layer play a critical role in the enhanced sensitivity and selectivity of the developed sensor towards Hg0 vapor. PMID:25338965

Methanol is a public health concern due to its toxicity, characterized by metabolic acidosis and blindness, among others. The third world population affected by the exposure to this compound is increasing, mainly due to the consumption of illicit distilled or adulterated alcoholic beverages. Although methanol is naturally present in some alcoholic drinks, the maximum allowed concentration cannot exceed 10 g of methanol per liter of anhydrous alcohol (0.4% (v/v) at 40% of ethanol) according to the general EU limit. A wireless passive microsensor was designed to detect small amounts of methanol at 40% of alcoholic dissolutions. The sensor consists of a planar inductor in series with an interdigital capacitor that changes its capacitance with the solution's dielectric constant. An antenna is used to readout the real part of the impedance to obtain the resonant frequencies for different amounts of methanol in the solution. The aim of this work was to develop a low cost wireless sensor with the capability to detect concentrations of at least 0.4% (v/v) of methanol in a 40% of alcoholic solution. The results obtained show variations of 403 kHz in the resonant frequency for changes of 0.2% (v/v) on the concentration of methanol in a 40% alcoholic ethanol-based solution. This project was possible thanks to the collaboration of the Department of Electrical and Electronics Engineering and the Department of Chemical Engineering of Universidad de los Andes.

Oxygen released by the roots of submerged plants may oxidize organic compounds from the roots and reduced substances continuously supplied by diffusion from the surrounding anoxic hydrosoil. We provide here the first visualization of this gradient environment obtained by microsensor analysis of oxygen in the rhizosphere of the freshwater plant Littorella uniflora (L.) Ascherson. The plants were rooted in an agar medium, in which amorphous FeS provided the main oxygen sink. The oxygen concentration at the root surface ranged from 20 to 450 [mu]M (atmospheric saturation = 280 [mu]M) between darkness and saturating light, and the oxic shell surrounding the roots varied from about 0.5 to 5 mm in thickness. The oxygen flux from the roots was a saturating function of the incident light intensity on the leaves, and the oxygen released was consumed mainly at the fluctuating oxic/anoxic interface. The oxic zones around individual roots are under dynamic control by light, root morphology, root density, and sediment reducing capacity, and, therefore, oxygen concentrations should be subject to substantial diurnal fluctuations in dense Littorella populations in nutrient-poor sediments. PMID:12232247

The performance of a novel prototype instrument in determining solvents and solvent mixtures permeating through samples of chemical protective clothing (CPC) materials was evaluated. The instrument contains a mini-preconcentrator and an array of three polymer-coated surface-acoustic-wave (SAW) microsensors whose collective response patterns are used to discriminate among multiple permeants. Permeation tests were performed with a 2.54 cm diameter test cell in an open-loop configuration on samples of common glove materials challenged with four individual solvents, three binary mixtures, and two ternary mixtures. Breakthrough times, defined as the times required for the permeation rate to reach a value of 1 microg cm(-2) min(-1), determined by the instrument were within 3 min of those determined in parallel by manual sampling and gas chromatographic analysis. Permeating solvents were recognized (identified) from their response patterns in 59 out of 64 measurements (92%) and their vapor concentrations were quantified to an accuracy of +/- 31% (typically +/- 10%). These results demonstrate the potential for such instrumentation to provide semi-automated field or bench-top screening of CPC permeation resistance. PMID:11249783

Commercial and military launch vehicles are designed to use cryogenic hydrogen as the main propellant, which is very volatile, extremely flammable, and highly explosive. Current detection system uses Teflon transfer tubes at small number of vehicle location through which gas samples are drawn and stream analyzed by a mass spectrometer. A concern with this approach is the high cost of the system. Also, the current system does not provide leak location and is not in real time. This system is very complex and cumbersome for production and ground support measurement personnel. This paper describes the successful test of a multipoint fiber optic hydrogen microsensors system on the Linear Aerospike X-33 rocket engine at NASA's Stennis Flight Center. The system consisted of a reversible chemical interaction causing a change in reflective of a thin film of coated Palladium. The sensor using a passive element consisting of chemically reactive microcoatings deposited on the surface of a glass microlens, which is then bonded to an optical fiber. The system uses a multiplexing technique with a fiber optic driver-receiver consisting of a modulated LED source that is launched into the sensor, and photodiode detector that synchronously measures the reflected signal. The system incorporates a microprocessor to perform the data analysis and storage, as well as trending and set alarm function. The paper illustrates the sensor design and performance data under field deployment conditions.

A reservoir type of capillary microsensor for pCO(2) measurements is presented. The sensor is based on the measurement of the fluorescence intensity of the anionic form of the pH indicator 1-hydroxy-3,6,8-pyrenetrisulfonate in the form of its ion pair with a quaternary ammonium base in an ethyl cellulose matrix. The glass capillary containing the reservoir sensor was prepared by immersing the tip of the optical fiber into the sensing agent very close to the sensor tip thus providing a very small volume for the sensing reaction. The purpose of the sensing approach is to regenerate the dye/buffer system by diffusion, which may be poisoned by interfering acids, or bleach by photolysis. The fresh cocktail from the reservoir takes the place of protonated form of the dye. The internal buffer system also makes the protonation-deprotonation equilibria reversible. The distal tip of the internal buffer containing reservoir is coated with a gas-permeable but ion-impermeable teflon membrane. The dynamic range for the detection of pCO(2) is between 1 and 20 hPa, which corresponds to the range of dissolved CO(2) in water. The response time is 15 s and the detection limit is 1 hPa of pCO(2.) The recovery performance of this sensor can be improved by means of mechanical adjustment of the sensor tip in a micrometric scale. PMID:18968907

The voltammetric oxidation in aqueous 0.1 Molar perchloric acid of four polyhydric alcohols, ethylene glycol, glycerol, meso-erythritol, and d-mannitol, on seven oriented gold surfaces is reported with the objective of assessing the role of surface crystallographic orientation on the catalytic electrooxidation of such poly-functional reactants. The automatically well-ordered nature of these gold surfaces has been scrutinized by in-situ scanning tunneling microscopy. In particular, the Au(221) and (533) faces were selected since they provide stepped surfaces, 4(111)-(111) and 4(111)-(100), respectively. The results are compared with corresponding data for simple unifunctional reactants, specifically for formic acid oxidation and with results reported previously for carbon monoxide oxidation. In contrast to the last reaction, the electrooxidation rates for both the polyhydric alcoholic and formic acid are greatest on Au(111), with Au(110) displaying unusually low activity. While formic acid electrooxidation is insensitive to the presence of monoatomic surface steps, the polyhydric alcohols (especially mannitol) are substantially less reactive on AU(221) and (533) relative to Au(111).

The ternary system of boric acid, salicylaldehyde (SA) and H-acid (HA) was voltammetrically studied from kinetic and equilibrium points of view. The effect of the SA substituents was also studied by using two analogs, 5-fluorosalicylaldehyde (F-SA) and 5-methylsalicylaldehyde (Me-SA). The three cathodic peaks of Azomethine H (AzH), Azomethine H-boric acid complex (AzB), and free SA were observed in the solution containing boric acid, SA and HA. The peak potentials of AzH and SA were shifted to negative potentials with increasing pH, while the peak potential of AzB was pH-independent. This difference indicates that a proton participates in the charge-transfer steps of the AzH and SA reductions, but not in that of the AzB reduction. The formation constants for the AzB complexation were similar among all the examined analogs. In the kinetic study, the reaction rate was higher in an acidic condition for the AzH formation, but in a neutral condition for the AzB formation. The rate constants for the AzB complexes were in the order of F-SA > SA ≈ Me-SA, indicating that the fluoro group accelerates the F-AzB complexation. The AzB complexation mechanism is considered to consist of more than three steps, i.e., the pre-equilibrium of the salicylaldehyde-boric acid complex (SA-B) formation, the nucleophilic attack of HA on SA-B, and the remaining some steps to form AzB. Based on these results, the voltammetric determination method of boron using F-SA was optimized, which allowed the boron concentration to be determined within only 5 min with a 0.03 mg B dm(-3) detection limit. PMID:25584642

Black tea is an extensively consumed beverage worldwide with an expanding market. The final quality of black tea depends upon number of chemical compounds present in the tea. Out of these compounds, theaflavins (TF), which is responsible for astringency in black tea, plays an important role in determining the final taste of the finished black tea. The present paper reports our effort to correlate the theaflavins contents with the voltammetric and potentiometric electronic tongue (e-tongue) data. Noble metal-based electrode array has been used for collecting data though voltammetric electronic tongue where as liquid filled membrane based electrodes have been used for potentiometric electronic tongue. Black tea samples with tea taster score and biochemical results have been collected from Tea Research Association, Tocklai, India for the analysis purpose. In this paper, voltammetric and potentiometric e-tongue responses are combined to demonstrate improvement of cluster formation among tea samples with different ranges of TF values.

A novel bionanocomposite, horse radish peroxidase- gold-nanoparticle-Calcium carbonate (HRP-AuNPs-CaCO3), hybrid material was encapsulated by silica sol on a glassy carbon electrode (GCE). The fabricated modified electrode was used as a novel voltammetric sensor for electrochemical sensing of anti-HIV replication drug i.e. deferiprone. The surface morphology of the modified electrode was characterized by scanning electron microscopy (SEM). Results obtained from the voltammetric measurements show that HRP-AuNPs-CaCO3 modified GCE offers a selective and sensitive electrochemical sensor for the determination of deferiprone. Under experimental conditions, the proposed voltammetric sensor has a linear response range from 0.01 to 10,000 μM with a detection limit of 0.01 μM. Furthermore, the fabricated sensor was successfully applied to determine deferiprone level in spiked urine and serum samples. PMID:25416586

Investigation of the electrochemical behavior using cyclic voltammetry and detection of [Mn2+(thiophenyl-2-carboxylic acid)2 (triethanolamine)] with adsorptive stripping differential pulse voltammetry. The electrochemical behavior of a manganese(II) complex [Mn2+(thiophenyl-2-carboxylic acid)2(triethanolamine)] (A) was investigated using cyclic and differential pulse voltammetry in an acetate buffer of pH 4.6 at a carbon paste electrode. Further, an oxidation–reduction mechanism was proposed. Meanwhile, an adsorptive stripping differential pulse voltammetric method was developed for the determination of manganese(II) complex. PMID:26819548

An inexpensive multielectrode voltammetry system designed for in vivo neurochemical studies of the awake, unanesthetized primate has been developed. Consisting of an Apple II Plus microcomputer, parallel operational amplifier circuitry for six working electrodes, and commercially available interface boards, the system has the flexibility to implement many standard voltammetric procedures under total software control. Multielectrode monitoring is accomplished essentially simultaneously, and all channels are equipped with independent gain controls allowing for rapid amplification adjustment. An interactive chronoamperometry program, capable of making rapid 12 bit analog to digital conversions for each working electrode over four software selectable ranges, is described and system performance is evaluated. PMID:6133600

This paper describes preliminary results in the development of an acoustic wave (SAW) microsensor array. The array is based on a novel configuration that allows for three sensors and a phase reference. Two configurations of the integrated array are discussed: a hybrid multichip-module based on a quartz SAW sensor with GaAs microelectronics and a fully monolithic GaAs-based SAW. Preliminary data are also presented for the use of the integrated SAW array in a gas-phase chemical micro system that incorporates microfabricated sample collectors and concentrators along with gas chromatography (GC) columns.

Critical micelle concentrations (cmc) of cetyltrimethylammonium bromide (CTAB) and cetylpyridinium chloride (CPC) surfactants in aqueous solution have been determined by using the cyclic voltammetric technique. (Co(en){sub 3})(ClO{sub 4}){sub 3} has been used as the redox-active electrochemical probe. The cmc values so obtained for the surfactants were found to be in good agreement with the literature values. The partition coefficient, K, of the electrochemical probe between water and surfactants in nonmicellar and micellar states was estimated using the peak current, i{sub p} and half-wave potential, E{sub 1/2} values. The self-diffusion coefficient, D{sub m}, interaction parameter, k{sub f}, and hydrodynamic radius of the micelles were also estimated. The results suggest that the probe is sensitive to the nature of surfactant as well as surfactant concentration.

This article describes the laboratory and field performance evaluation of a small prototype instrument employing an array of six polymer-coated surface acoustic wave (SAW) sensors and a thermal desorption preconcentration unit for rapid analysis of perchloroethylene in breath. Laboratory calibrations were performed using breath samples spiked with perchloroethylene to prepare calibration standards spanning a concentration range of 0.1-10 ppm. A sample volume of 250 mL was preconcentrated on 40 mg of Tenax GR at a flow rate of 100 mL/min, followed by a dry air purge and thermal desorption at a temperature of 200 degrees C. The resulting pulse of vapor was passed over the sensor array at a flow rate of 20 mL/min and sensor responses were recorded and displayed using a laptop computer. The total time per analysis was 4.5 min. SAW sensor responses were linear, and the instrument's limit of detection was estimated to be 50 ppb based on the criterion that four of the six sensors show a detectable response. Field performance was evaluated at a commercial dry-cleaning operation by comparing prototype instrument results for breath samples with those of a portable gas chromatograph (NIOSH 3704). Four breath samples were collected from a single subject over the course of the workday and analyzed using the portable gas chromatograph (GC) and SAW instruments. An additional seven spiked breath samples were prepared and analyzed so that a broader range of perchloroethylene concentrations could be examined. Linear regression analysis showed excellent agreement between prototype instrument and portable GC breath sample results with a correlation coefficient of 0.99 and a slope of 1.04. The average error for the prototype instrument over a perchloroethylene breath concentration range of 0.9-7.2 ppm was 2.6% relative to the portable GC. These results demonstrate the field capabilities of SAW microsensor arrays for rapid analysis of organic vapors in breath. PMID:15742707

Optical hydrogen sensors are intrinsically safe since they produce no arc or spark in an explosive environment caused by the leakage of hydrogen. Safety remains a top priority since leakage of hydrogen in air during production, storage, transfer and distribution creates an explosive atmosphere for concentrations between 4% (v/v) - the lower explosive limit (LEL) and 74.5% (v/v) - the upper explosive limit (UEL) at room temperature and pressure. Being a very small molecule, hydrogen is prone to leakage through seals and micro-cracks. Hydrogen detection in space application is very challenging; public acceptance of hydrogen fuel would require the integration of a reliable hydrogen safety sensor. For detecting leakage of cryogenic fluids in spaceport facilities, Launch vehicle industry and aerospace agencies are currently relying heavily on the bulky mass spectrometers, which fill one or more equipment racks, and weigh several hundred kilograms. This paper describes the successful development and test of a multi-point fiber optic hydrogen sensor system during the static firing of an Evolved Expandable Launch Vehicle at NASA's Stennis Space Center. The system consisted of microsensors (optrodes) using hydrogen gas sensitive indicator incorporated onto an optically transparent porous substrate. The modular optoelectronics and multiplexing network system was designed and assembled utilizing a multi-channel optoelectronic sensor readout unit that monitored the hydrogen and temperature response of the individual optrodes in real-time and communicated this information via a serial communication port to a remote laptop computer. The paper would discuss the sensor design and performance data under field deployment conditions.

Indole-3-acetic acid (IAA) is a primary phytohormone that regulates multiple aspects of plant development. Because polar transport of IAA is an essential determinant of organogenesis and dynamic tropic growth, methods to monitor IAA movement in vivo are in demand. A self-referencing electrochemical microsensor was optimized to non-invasively measure endogenous IAA flux near the surface of Zea mays roots without the addition of exogenous IAA. Enhanced sensor surface modification, decoupling of acquired signals, and integrated flux analyses were combined to provide direct, real time quantification of endogenous IAA movement in B73 maize inbred and brachytic2 (br2) auxin transport mutant roots. BR2 is localized in epidermal and hypodermal tissues at the root apex. br2 roots exhibit reduced shootward IAA transport at the root apex in radiotracer experiments and reduced gravitropic growth. IAA flux data indicates that maximal transport occurs in the distal elongation zone of maize roots, and net transport in/out of br2 roots was decreased compared to B73. Integration of short term real time flux data in this zone revealed oscillatory patterns, with B73 exhibiting shorter oscillatory periods and greater amplitude than br2. IAA efflux and influx were inhibited using 1-N-naphthylphthalamic acid (NPA), and 2-naphthoxyacetic acid (NOA), respectively. A simple harmonic oscillation model of these data produced a correlation between modeled and measured values of 0.70 for B73 and 0.69 for br2. These results indicate that this technique is useful for real-time IAA transport monitoring in surface tissues and that this approach can be performed simultaneously with current live imaging techniques. PMID:20626658

Knowledge of mass transport mechanisms in biofilm-based technologies such as biofilters is essential to improve bioreactors performance by preventing mass transport limitation. External and internal mass transport in biofilms was characterized in heterotrophic biofilms grown on a flat plate bioreactor. Mass transport resistance through the liquid-biofilm interphase and diffusion within biofilms were quantified by in situ measurements using microsensors with a high spatial resolution (<50 μm). Experimental conditions were selected using a mathematical procedure based on the Fisher Information Matrix to increase the reliability of experimental data and minimize confidence intervals of estimated mass transport coefficients. The sensitivity of external and internal mass transport resistances to flow conditions within the range of typical fluid velocities over biofilms (Reynolds numbers between 0.5 and 7) was assessed. Estimated external mass transfer coefficients at different liquid phase flow velocities showed discrepancies with studies considering laminar conditions in the diffusive boundary layer near the liquid-biofilm interphase. The correlation of effective diffusivity with flow velocities showed that the heterogeneous structure of biofilms defines the transport mechanisms inside biofilms. Internal mass transport was driven by diffusion through cell clusters and aggregates at Re below 2.8. Conversely, mass transport was driven by advection within pores, voids and water channels at Re above 5.6. Between both flow velocities, mass transport occurred by a combination of advection and diffusion. Effective diffusivities estimated at different biofilm densities showed a linear increase of mass transport resistance due to a porosity decrease up to biofilm densities of 50 g VSS·L(-1). Mass transport was strongly limited at higher biofilm densities. Internal mass transport results were used to propose an empirical correlation to assess the effective diffusivity

Hydrologic and water quality observatories are being planned with a vision of enhancing our ability to better understand, forecast and adaptively manage both water quantity and quality. To adequately cover these spatially and temporally variable systems, distributed, embedded sensor networks must be designed with the proper mix (multimodality) of sensors to quantify key system properties, including temperature and chemical distributions, as well as mass and energy fluxes, and to do so across multiple scales. Given resource limitations, process models need to be coupled to the sensor network to interpolate between sensor data. This work focuses on the spatially distributed flux of nutrients, specifically nitrate, in surface-subsurface environments. It begins at the sensor level, describing the development and testing of nitrate microsensors that are scaleable to large, dense sensor networks required to cover heterogeneous watersheds, including associated soil and sediment systems. First and second generation miniature and inexpensive nitrate sensors (ion selective electrodes) fabricated by depositing conducting polymers on carbon substrates are presented in the context of laboratory and field tests. While these sensors are limited to relatively short deployments (4-8 weeks), there are potential strategies for overcoming this problem. Scale-up to one- and three-dimensional soil/sediment sensor arrays is discussed in the context of two deployments: (1) a groundwater quality protection network, where recycled wastewater that is potentially high in nitrate is being used for agricultural irrigation, and (2) nonpoint source nitrate pollution in rivers and groundwater in agricultural watersheds. Recent hardware (wireless transceivers) and software advancements (e.g., network topology design and debugging, energy management) intended for networks spanning 100s of m in space are outlined in these examples. The discussion extends to sensor form factor, in situ calibration

This paper summarises the results of voltammetric studies on the herbicide 3-(3,4-dichlorophenyl)-1-methoxy-1-methylurea (Linuron), using a carbon paste electrode containing tricresyl phosphate (TCP-CPE) as liquid binder. The principal experimental conditions, such as the pH effect, investigated in Britton-Robinson buffer solutions (pH 2.0–7.0), the peak characteristics for the analyte of interest, or instrumental parameters for the differential pulse voltammetric mode were optimized for the method. As found out, the best electroanalytical performance of the TCP-CPE was achieved at pH 2.0, whereby the oxidation peak of Linuron appeared at ca. +1.3 V vs. SCE. The analytical procedure developed offers good linearity in the concentration range of 1.25–44.20 μg mL−1 (1.77 × 10−4–5.05 × 10−6 mol L−1), showing—for the first time—the applicability of the TCP-CPE for anodic oxidations in direct voltammetry (without accumulation). The method was then verified by determining Linuron in a spiked river water sample and a commercial formulation and the results obtained agreed well with those obtained by the reference HPLC/UV determination. PMID:22368461

The preparation and electrochemical characterization of a nickel hydroxide modified nickel electrode as well as its behavior as electrocatalyst toward the oxidation of hydrochlorothiazide (HCTZ) were investigated. The electrochemical behavior of the modified electrode and the electrooxidation of HCTZ were explored using cyclic voltammetry. The voltammetric response of the modified electrode in the detection of HCTZ is based on the electrochemical oxidation of the Ni(II)/Ni(III) and a chemical redox process. The analytical parameters for the electrooxidation of HCTZ by the nickel hydroxide modified nickel electrode were obtained in NaOH solution, in which the linear voltammetric response was in the concentration range from 1.39×10(-5) to 1.67×10(-4)mol L(-1) with a limit of detection of 7.92×10(-6)mol L(-1) and a sensitivity of 0.138 μA Lmmol(-1). Tafel analysis was used to elucidate the kinetics and mechanism of HCTZ oxidation by the modified electrode. PMID:26354274

This work describes the construction and application of carbon paste electrodes modified with biochar and antimony microparticles (SbBCPE) for voltammetric determination of paraquat using a simple and sensitive procedure based on voltammetric stripping analysis. Some parameters such as amount of biochar and antimony used in the composition of the carbon paste and instrumental parameters were examined in detail. Under optimized conditions, an analytical curve was obtained for paraquat determination employing SbBCPE, which showed a linear response ranging from 0.2 to 2.9 μmol L(-1), with limit of detection and quantification of 34 nmol L(-1) and 113 nmol L(-1), respectively, after paraquat pre-concentration of 120 s. The repeatability study presented a RSD=2.0% for 10 consecutive measurements using the same electrode surface and the reproducibility study showed a RSD=2.7% for measurements with 10 different electrode surfaces. The proposed sensor was successfully applied for paraquat determination in tap water and citric fruit juice spiked samples and good recoveries were obtained without any sample pre-treatment, showing its promising analytical performance. PMID:26952405

The temperature dependence of the electroactive polymer film voltammetric response is considered under conditions of surface or thin-layer behavior. Existing theory is used to show how information regarding the variation of the electrode process with temperature and the transition between thin-layer and diffusion behavior can be obtained from experimental data. Poly(vinylferrocene) (PVF) and tetracyanoquinodimethane (TCNQ) polymer modified electrodes have been studied under the following conditions: PVF/CH/sub 3/CN/0.1M (C/sub 2/H/sub 5/)/sub 4/NClO/sub 4/, -30 to 50/sup 0/C; and TCNQ/aqueous pH 7 buffer, 2.5 to 55/sup 0/C. For the PVF electrodes the interaction parameter extracted for the wave shape of the surface voltammograms decreased markedly at the lower temperatures. For both systems it is suggested that the temperature dependence of the voltammetric response is strongly influenced by solvent swelling of the polymer film. 29 references, 5 figures, 3 tables.

In this study, a new selective and sensitive voltammetric procedure for determination of acyclovir (ACV) was proposed using a disposable electrode, pencil graphite electrode (PGE). Cyclic and differential pulse voltammograms of ACV were recorded in Britton-Robinson buffer solution containing 0.10 M KCl with pH of 4.0 at PGE. The PGE displayed a very good electrochemical behavior with significant enhancement of the peak current compared to a glassy carbon electrode (GCE). Under experimental conditions, the PGE had a linear response range from 1.0 μM to 100.0 μM ACV with a detection limit of 0.3 μM (based on 3 Sb). Relative standard deviations of 4.8 and 3.6% were obtained for five successive determinations of 10.0 and 50.0 μM ACV, respectively, which indicate acceptable repeatability. This voltammetric method was successfully applied to the direct determination of ACV in real pharmaceutical samples. The effect of various interfering compounds on the ACV peak current was studied. PMID:27040252

A novel vapor permeation-stepwise injection (VP-SWI) method for the determination of methanol and ethanol in biodiesel samples is discussed. In the current study, stepwise injection analysis was successfully combined with voltammetric detection and vapor permeation. This method is based on the separation of methanol and ethanol from a sample using a vapor permeation module (VPM) with a selective polymer membrane based on poly(phenylene isophtalamide) (PA) containing high amounts of a residual solvent. After the evaporation into the headspace of the VPM, methanol and ethanol were transported, by gas bubbling, through a PA membrane to a mixing chamber equipped with a voltammetric detector. Ethanol was selectively detected at +0.19 V, and both compounds were detected at +1.20 V. Current subtractions (using a correction factor) were used for the selective determination of methanol. A linear range between 0.05 and 0.5% (m/m) was established for each analyte. The limits of detection were estimated at 0.02% (m/m) for ethanol and methanol. The sample throughput was 5 samples h(-1). The method was successfully applied to the analysis of biodiesel samples. PMID:26653499

This work reports the application of a voltammetric electronic tongue system (ET) made from an array of modified graphite-epoxy composites plus a gold microelectrode in the qualitative and quantitative analysis of polyphenols found in wine. Wine samples were analyzed using cyclic voltammetry without any sample pretreatment. The obtained responses were preprocessed employing discrete wavelet transform (DWT) in order to compress and extract significant features from the voltammetric signals, and the obtained approximation coefficients fed a multivariate calibration method (artificial neural network-ANN-or partial least squares-PLS-) which accomplished the quantification of total polyphenol content. External test subset samples results were compared with the ones obtained with the Folin-Ciocalteu (FC) method and UV absorbance polyphenol index (I(280)) as reference values, with highly significant correlation coefficients of 0.979 and 0.963 in the range from 50 to 2400 mg L(-1) gallic acid equivalents, respectively. In a separate experiment, qualitative discrimination of different polyphenols found in wine was also assessed by principal component analysis (PCA). PMID:22688049

The electrochemical sensing of new psychoactive substances, synthetic cannabinoids (SCs), commonly marketed under the trade name "Spice" is explored for the first time. The electrooxidative transformations of 11 new indole and indazole SCs which are currently the predominant illicit smoking mixtures on the drug market is performed using cyclic and differential pulse voltammetry with various commercially available electrodes (Pt, GC, Bdd). It is found that SCs exhibit voltammetric responses that can be used for their detection in smoking mixtures and artificial saliva with limits of detection in the nanomolar range. The indole-based SCs exhibited an anodic peak at ∼1.5 V (vs Ag/Ag(+)) and ∼1.2 V (vs Ag/AgCl) in acetonitrile and artificial saliva, respectively, and the indazoles exhibited corresponding peaks at ∼1.7 V and ∼1.5 V. The voltammetric procedure was evaluated by prescreening of SCs in 12 confiscated street samples that were also independently analyzed by GC-MS and LC-MS techniques. A good agreement between the three analytical protocols was found. Voltammetry provides a tool for the prescreening of synthetic cannabinoid derivatives in seized materials and biological samples. PMID:26905258

Biofilms used in bioelectrochemical systems are expected to transfer electrons using electron transfer mediators. One mediator type, flavins, which includes flavin mononucleotide, riboflavin, and flavin adenine dinucleotide, has been found to be endogenously produced by Shewanella oneidensis MR-1. However, the presence and concentration of flavins inside a S. oneidensis MR-1 biofilm have never been reported. The goal of this study was to develop a flavin microelectrode capable of measuring flavins inside a living biofilm and apply it to a biofilm which produces flavins. Because flavins are electrochemically active molecules, the flavin microelectrode was based on detection via square-wave voltammetry. The microelectrode consisted of a carbon working electrode with a 10–30 μm tip diameter, a built-in platinum counter electrode, and a Ag/AgCl reference electrode, all enclosed in a glass outer case. The microelectrode was calibrated between 0.1 μM and 10 μM flavins and showed a linear correlation between flavin concentration and peak currents located at −424 mVAg/AgCl on a square-wave voltammogram. We also developed a model to explain the electrochemical mechanism of flavin detection, and to determine the effective surface area of the microelectrode, the standard reduction potential, and the transfer coefficient. We found that the effective surface area of the microelectrode was close to 100 times the projected surface area. The model predicted a standard reduction potential for RF/RFH2 of −419 mVAg/AgCl at 20 °C and a transfer coefficient of 0.45. Lastly, we measured flavin concentration inside a S. oneidensis MR-1 biofilm grown on a glass surface using oxygen as the electron acceptor. The flavin concentration reached 0.7 μM, increasing near the bottom of the biofilm, where no oxygen was present. This shows the possibility that flavins are produced in the anaerobic zone to act as intermediate electron acceptors in the deeper parts of the biofilm, where

Biofilms used in bioelectrochemical systems are expected to transfer electrons using electron transfer mediators. One mediator type, flavins, which includes flavin mononucleotide, riboflavin, and flavin adenine dinucleotide, has been found to be endogenously produced by Shewanella oneidensis MR-1. However, the presence and concentration of flavins inside a S. oneidensis MR-1 biofilm have never been reported. The goal of this study was to develop a flavin microelectrode capable of measuring flavins inside a living biofilm and apply it to a biofilm which produces flavins. Because flavins are electrochemically active molecules, the flavin microelectrode was based on detection via square-wave voltammetry. The microelectrode consisted of a carbon working electrode with a 10-30 μm tip diameter, a built-in platinum counter electrode, and a Ag/AgCl reference electrode, all enclosed in a glass outer case. The microelectrode was calibrated between 0.1 μM and 10 μM flavins and showed a linear correlation between flavin concentration and peak currents located at -424 mV(Ag/AgCl) on a square-wave voltammogram. We also developed a model to explain the electrochemical mechanism of flavin detection, and to determine the effective surface area of the microelectrode, the standard reduction potential, and the transfer coefficient. We found that the effective surface area of the microelectrode was close to 100 times the projected surface area. The model predicted a standard reduction potential for RF/RFH2 of -419 mV(Ag/AgCl) at 20 °C and a transfer coefficient of 0.45. Lastly, we measured flavin concentration inside a S. oneidensis MR-1 biofilm grown on a glass surface using oxygen as the electron acceptor. The flavin concentration reached 0.7 μM, increasing near the bottom of the biofilm, where no oxygen was present. This shows the possibility that flavins are produced in the anaerobic zone to act as intermediate electron acceptors in the deeper parts of the biofilm, where there

In this study, a cost-effective and highly sensitive cholesterol microsensor, which is consisted of cholesterol oxidase (ChOx), horseradish peroxidase (HRP), and polyaniline (PANI), was developed based on the enzyme-induced conductivity change of PANI with fast response. Hydrogen peroxide is produced via the reaction between cholesterol and ChOx, which was immobilized in a dialysis membrane. The produced hydrogen peroxide can oxidize HRP, which can be reduced by oxidizing PANI, thus resulting in decreased conductivity of the polyaniline thin film. The reduced HRP can be oxidized again by hydrogen peroxide and the cycle of the oxidation/reduction continues until all hydrogen peroxide are reacted, leading to the high sensitivity of the sensor due to the signal contributed from all hydrogen peroxide molecules. Cholesterol was detected near the physiological concentrations ranging from 100 mg/dl to 400 mg/dl with the cholesterol microsensors. The results show linear relation between cholesterol concentration and the conductivity change of the PANI. The microsensor showed no response to cholesterol when the PANI was standalone without cholesterol oxidase immobilized, indicating that the enzymatic reaction is required for cholesterol detection. The simple process of the sensor fabrication allows the sensor to be cost-effective and disposable usage. This electronic cholesterol microsensor is promising for point-of-care health monitoring in cholesterol level with low cost and fast response.

In this study, a cost-effective and highly sensitive cholesterol microsensor, which is consisted of cholesterol oxidase (ChOx), horseradish peroxidase (HRP), and polyaniline (PANI), was developed based on the enzyme-induced conductivity change of PANI with fast response. Hydrogen peroxide is produced via the reaction between cholesterol and ChOx, which was immobilized in a dialysis membrane. The produced hydrogen peroxide can oxidize HRP, which can be reduced by oxidizing PANI, thus resulting in decreased conductivity of the polyaniline thin film. The reduced HRP can be oxidized again by hydrogen peroxide and the cycle of the oxidation/reduction continues until all hydrogen peroxide are reacted, leading to the high sensitivity of the sensor due to the signal contributed from all hydrogen peroxide molecules. Cholesterol was detected near the physiological concentrations ranging from 100 mg/dl to 400 mg/dl with the cholesterol microsensors. The results show linear relation between cholesterol concentration and the conductivity change of the PANI. The microsensor showed no response to cholesterol when the PANI was standalone without cholesterol oxidase immobilized, indicating that the enzymatic reaction is required for cholesterol detection. The simple process of the sensor fabrication allows the sensor to be cost-effective and disposable usage. This electronic cholesterol microsensor is promising for point-of-care health monitoring in cholesterol level with low cost and fast response.

This article introduces a power-efficient, miniature electronic nose (e-nose) system. The e-nose system primarily comprises two self-developed chips, a multiple-walled carbon nanotube (MWNT)-polymer based microsensor array, and a low-power signal-processing chip. The microsensor array was fabricated on a silicon wafer by using standard photolithography technology. The microsensor array comprised eight interdigitated electrodes surrounded by SU-8 "walls," which restrained the material-solvent liquid in a defined area of 650 × 760 μm(2). To achieve a reliable sensor-manufacturing process, we used a two-layer deposition method, coating the MWNTs and polymer film as the first and second layers, respectively. The low-power signal-processing chip included array data acquisition circuits and a signal-processing core. The MWNT-polymer microsensor array can directly connect with array data acquisition circuits, which comprise sensor interface circuitry and an analog-to-digital converter; the signal-processing core consists of memory and a microprocessor. The core executes the program, classifying the odor data received from the array data acquisition circuits. The low-power signal-processing chip was designed and fabricated using the Taiwan Semiconductor Manufacturing Company 0.18-μm 1P6M standard complementary metal oxide semiconductor process. The chip consumes only 1.05 mW of power at supply voltages of 1 and 1.8 V for the array data acquisition circuits and the signal-processing core, respectively. The miniature e-nose system, which used a microsensor array, a low-power signal-processing chip, and an embedded k-nearest-neighbor-based pattern recognition algorithm, was developed as a prototype that successfully recognized the complex odors of tincture, sorghum wine, sake, whisky, and vodka. PMID:24385138

Background Atrazine (ATZ) is a widely used herbicide in most countries because of its low cost and good selectivity. The concentration of ATZ that the EPA considers safe to consume in drinking water is 3 ppb. Therefore, recently, there have been concerns about its determination in trace levels. This compound is not electro-active, so in this research indirect electrochemical method for its detection in low levels was proposed. Objectives The main aim of this study is the indirect determination of ATZ in water samples by voltammetry using nano-particle modified electrode. Materials and Methods A nano-CuO modified carbon paste electrode (NMCPE) is constructed and its application for indirect square wave voltammetric (SWV) detection of ATZ is reported. The sensing performance mechanism of the nano-CuO modified carbon paste electrode toward atrazine is due to complexation of the analyte with Cu (II) ion. The peak current for copper (II) reduction decreases with increase in the ATZ concentration and is monitored for its determination. Instrumental and chemical parameters influencing the detection of ATZ were optimized. Results The results revealed that decrease in peak current was proportional to ATZ concentration over the range of 5-75 ng/mL. The limit of detection (LOD) and limit of quantification (LOQ) were 2 ng/mL and 5.6 ng/mL (n = 20), respectively. The relative standard deviation (n = 10) for the determination of 10 and 50 ng/mL of ATZ solution was estimated as 4.9% and 4.2 %, respectively. Conclusions This easily fabricated electrode together with the fast and sensitive SW voltammetry was successfully applied for the determination of concentration of ATZ at trace levels, in different water samples. PMID:24624200

Three phenolic compounds, i.e. phenol, catechol and 4-acetamidophenol, were simultaneously determined by voltammetric detection of its oxidation reaction at the surface of an epoxy-graphite transducer. Because of strong signal overlapping, Wavelet Neural Networks (WNN) were used in data treatment, in a combination of chemometrics and electrochemical sensors, already known as the electronic tongue concept. To facilitate calibration, a set of samples (concentration of each phenol ranging from 0.25 to 2.5mM) was prepared automatically by employing a Sequential Injection System. Phenolic compounds could be resolved with good prediction ability, showing correlation coefficients greater than 0.929 when the obtained values were compared with those expected for a set of samples not employed for training. PMID:18585293

This work presents a complete methodology of distinguishing between different brands of cider and ageing degrees, based on voltammetric signals, utilizing dedicated data preprocessing procedures and unsupervised multivariate analysis. It was demonstrated that voltammograms recorded on glassy carbon electrode in Britton-Robinson buffer at pH 2 are reproducible for each brand. By application of clustering algorithms and principal component analysis visible homogenous clusters were obtained. Advanced signal processing strategy which included automatic baseline correction, interval scaling and continuous wavelet transform with dedicated mother wavelet, was a key step in the correct recognition of the objects. The results show that voltammetry combined with optimized univariate and multivariate data processing is a sufficient tool to distinguish between ciders from various brands and to evaluate their freshness. PMID:26948640

The adsorption properties of dioxouranium (II)-Phathalate complexes onto hanging mercury drop electrode are exploited in developing a highly sensitive and selective stripping voltammetric procedure for the determination of uranium (VI). The reduction current of adsorbed complex ions of U(VI) was measured by both linear sweep (LSCSV) and differential pulse cathodic stripping voltammetry (DPCSV), preceded by a period of preconcentration onto the electrode surface. As low as 2x10(-9) mol dm(-3) (0.5 mug/l) and 2x10(-8) mol dm(-3) (4.8 mug/l) with accumulation time 240 and 120 s using DPCSV and LSCSV, respectively, have been determined successfully. The relative standard deviation of 2.2% at the 5 ppm level was obtained. The interferences of some metal ions and anions were studied. The application of this method was tested in the determination of uranium in superphosphate fertilizer. PMID:18967571

A new automated batch method for the determination of ultratrace metals (nanogram per liter level) was developed and validated. Instrumental and chemical parameters affecting the performance of the method were carefully assessed and optimized. A wide range of voltammetric methods under different chemical conditions were tested. Cadmium, lead and copper were determined by anodic stripping voltammetry (ASV), while nickel, cobalt, rhodium and uranium by adsorptive cathodic stripping voltammetry (AdCSV). The figures of merit of all of these methods were determined: very good precision and accuracy were achieved, e.g. relative percentage standard deviation in the 4-13% for ASV and 2-5% for AdCSV. The stripping methods were applied to the determination of cadmium, lead, copper, nickel, cobalt, rhodium and uranium in lake water samples and the results were found to be comparable with ICP-MS data. PMID:17586114

A fully integrated wireless inductance-capacitance (LC) coupling microsensor was designed and fabricated by MEMS technology. The sensing loop was formed by connecting a deformable parallel-plated capacitor and a planar spiral inductor with a Ni(80)Fe(20) core. Polyimide and PMMA were used to isolate and package the devices. Typical dimension of the sensors was 5 × 5 mm2 × 0.77 mm. Different electroplated inductive coils (30, 40, and 60 turns) were fabricated to connect with a 4 × 4 mm2 plate capacitor in series. The LC sensing module for measuring liquid-level induced frequency responses was setup. Experimental results show that frequency response decreased as liquid level increased and sensitivity is about 7.01 kHz/cm with deviation less than 2%. Developed planar spiral inductor with high permeability magnetic core can provide a wide range of frequency variation in LC sensing applications.

In this paper is presented an overview of the technological barriers faced by the in vivo brain analysis with microelectrodes. Numerous microsensors and enzymatic microbiosensors have been developed for the real time monitoring of neurotransmitters, neuromodulators, drugs and diverse other biological relevant substances. A clear understanding of the working principle, advantages and limitations is essential for the acquisition of valid data in neurological investigations. Some of the aspects presented here refer to: microelectrode insertion and positioning related to possibilities to minimize tissue damage, spatial and temporal resolution of the measurements, actual controversies in data interpretation and sensor calibration, simultaneous detection of multiple analytes, interferences and state of the art in the development of wireless devices. PMID:23449399

Finite-element based computational simulation is performed to investigate the effect of an electrical double layer (EDL) on the electrochemical processes of nanometer-scale interdigitated electrodes (nano-IDEs). Results show that the EDL structure will alter the voltammetric current response of nano-IDEs due to the expansion of the diffuse layer into the diffusion layer at the electrode surfaces and the overlap of the electrical fields of the neighboring electrodes. The EDL induced change in the voltammetric current response is more severe for nano-IDEs with a smaller electrode size and gap spacing, and the EDL effect is influenced by the compact layer thickness, the charge valence of the redox species, the electron transfer rate, and the absence of the supporting electrolyte.

This paper describes the development of an electrochemical assay based on screen-printed carbon sensors for the determination of clonazepam in serum and in wine. The cyclic voltammetric behaviour of the drug was investigated and the effects of pH and scan rate on the peak current and peak potential determined. Two reduction peaks were recorded on the initial negative going scan, which were considered to result from the 2e(-), 2 H(+) reduction of the 4,5-azomethine and from the 4e(-), 4 H(+) reduction of the 7-NO2 to a hydroxylamine. On the return positive going scan an oxidation peak was seen, which was considered to result from the 2e(-), 2 H(+) oxidation (O1) of the hydroxylamine to the corresponding nitroso species. At pH 11 the solution of clonazepam was found to turn from clear to yellow in colour and the voltammetric signal of the O1 oxidation process was found to be adsorptive in nature, this was exploited in the development of an adsorptive stripping voltammetric assay. Experimental conditions were then optimised for the differential pulse adsorptive voltammetric measurement of clonazepam in wine and serum samples. It was shown that these analyses could be performed on only 100µL of sample which was deposited on the sensor surface. Mean recoveries of 79.53% (%CV=9.88%) and 88.22% (%CV=14.1%) were calculated for wine fortified with 3.16µg/mL and serum fortified with 12.6µg/mL. PMID:26592640

Qualitative and quantitative electrochemical methods for trace ion analysis of organic and inorganic species with environmental and biological attention have been developed and reported during past decades. The development of fast and accurate electrochemical methods is critical for field applications with various blocking contaminants. Voltammetric method is attractive not only to analyze selective ion species due to its characteristic based on ion lipophilicity, but also to lower the limit of detection by combining with stripping analysis. In my PhD work, I have developed and studied a highly selective and sensitive electrochemical method that can be used to characterize fundamental transport dynamics and to develop electrochemical sensors at liquid/liquid interfaces based on electrochemically-controlled ion transfer and recognition. The understanding of the kinetic and thermodynamic properties of the voltammetric ion transfer through polymer-modified ion-selective electrodes leads to realize the highly selective and sensitive analytical method. The ultrathin polymer membrane is used to maximize a current response by complete exhaustion of preconcentrated ions. Therefore, nanomolar detection is achieved and confirmed by a thermodynamic mechanism that controls the detection limit. It was also demonstrated experimentally and theoretically that more lipophilic ionic species gives a significantly lower detection limit. The voltammetric method was expanded into inexpensive and disposable applications based on pencil lead modified with the thin polymer membrane. In the other hand, micropipet/nanopipet voltammetry as an artificial cell membrane was used to study the interface between two immiscible solutions for environmental and biomedical applications. It is very useful to get quantitative kinetic and thermodynamic information by studying numerical simulations of ion transfer and diffusion. Molecular recognition and transport of heparin and low

A new method based on the Butler-Volmer formalism is applied to assess the capability of two voltammetric ion sensors based on polypyrrole films: PPy/DBS and PPy/ClO4 modified electrodes were studied as voltammetric cation and anion sensors, respectively. The reversible potential versus electrolyte concentrations semilogarithm plots provided positive calibration slopes for PPy/DBS and negative ones for PPy/ClO4, as was expected from the proposed method and that based on the Nernst equation. The slope expressions deduced from Butler-Volmer include the electron-transfer coefficient, which allows slope values different from the ideal Nernstian value to be explained. Both polymeric films exhibited a degree of ion-selectivity when they were immersed in mixed-analyte solutions. Selectivity coefficients for the two proposed voltammetric cation and anion sensors were obtained by several experimental methods, including the separated solution method (SSM) and matched potential method (MPM). The K values acquired by the different methods were very close for both polymeric sensors. PMID:19367868

Lithium batteries are widely used in notebook computers, mobile phones, 3C electronic products, and electric vehicles. However, under a high charge/discharge rate, the internal temperature of lithium battery may rise sharply, thus causing safety problems. On the other hand, when the lithium battery is overcharged, the voltage and current may be affected, resulting in battery instability. This study applies the micro-electro-mechanical systems (MEMS) technology on a flexible substrate, and develops a flexible three-in-one microsensor that can withstand the internal harsh environment of a lithium battery and instantly measure the internal temperature, voltage and current of the battery. Then, the internal information can be fed back to the outside in advance for the purpose of safety management without damaging the lithium battery structure. The proposed flexible three-in-one microsensor should prove helpful for the improvement of lithium battery design or material development in the future. PMID:25996509

Lithium batteries are widely used in notebook computers, mobile phones, 3C electronic products, and electric vehicles. However, under a high charge/discharge rate, the internal temperature of lithium battery may rise sharply, thus causing safety problems. On the other hand, when the lithium battery is overcharged, the voltage and current may be affected, resulting in battery instability. This study applies the micro-electro-mechanical systems (MEMS) technology on a flexible substrate, and develops a flexible three-in-one microsensor that can withstand the internal harsh environment of a lithium battery and instantly measure the internal temperature, voltage and current of the battery. Then, the internal information can be fed back to the outside in advance for the purpose of safety management without damaging the lithium battery structure. The proposed flexible three-in-one microsensor should prove helpful for the improvement of lithium battery design or material development in the future. PMID:25996509

Microsensors do not have the selectivity to chemical species available in large laboratory instruments. This project employed arrays of catalytically gated silicon microsensors with different catalysts to create data streams which can be analyzed by pattern recognition programs. One of the most significant accomplishments of the program was the demonstration of that mixtures of H{sub 2} with the oxidants NO{sub x} and O{sub 2} could distinguished from one another by the use of different catalytic metals on the Sandia Robust Hydrogen (SRH) sensors and the newly developed pattern recognition algorithm. This sensor system could be used to identify explosive gas mixtures and analyze exhaust streams for pollution control.

Microelectrodes of silver-copper alloys have been evaluated for use in voltammetric analyses. Increased overpotential towards the hydrogen overvoltage reaction (HER) was found as a function of increased copper content in the silver. A study of oxidizing products by cyclic voltammetry (CV) in NaOH solution showed ten anodic and eight cathodic peaks which are described in the present paper. The behaviour of these alloy electrodes is somewhere between pure silver and pure copper electrodes. Differential pulse anodic stripping voltammetry (DPASV) was used to measure zinc, cadmium and lead in ultrapure water only (18 MOmegacm), and good linearity was found for all metals (r (2)=0.998) in the range of 0.5 to 5 ppb with a 600- to 1,200-s plating time. It was additionally found that cadmium and lead were better separated on the alloy electrodes compared to pure silver electrodes. Measurements of nickel were carried out on alloy electrodes by use of adsorptive differential pulse cathodic stripping voltammetry (Ad-DPCSV), and good linearity (r (2)=1.000) was found in the range from 0.5 to 5 ppb with an adsorption time of 120 s. The alloy electrodes were also found to be sensitive to nitrate, and good linearity (r (2)=0.997) was found in the range from 1 mg L(-1) to 100 mg L(-1) using differential pulse voltammetry (DPV) scanning from -450 mV to -1,500 mV. Addition of nitrate in ultrapure water afforded two different peaks related to the successive reductions of nitrate and nitrite. In ammonium buffer solution (pH 8.6) only one peak resulting from reduction of nitrate was observed. Furthermore, the use of alloy electrodes containing 17% Cu was tested in real samples, by installing it in a voltammetric system for monitoring of zinc and lead in a polluted river, the river Deûle, near the town of Douai in northern France. Results were found to be in agreement with parallel measurements carried out by ICP-MS. PMID:16550424

Stripping voltammetry as technique has proved to be very useful in the analysis of heavy and other metal ions due to its excellent detection limits and its sensitivity in the presence of different metal species or interfering ions. Recent assessments of aquatic samples have shown increased levels of platinum group metals (PGMs) in aquatic ecosystems, caused by automobile exhaust emissions and mining activities. The development of an analytical sensor for the detection and characterisation of PGMs were investigated, since there is an ongoing need to find new sensing materials with suitable recognition elements that can respond selectively and reversibly to specific metal ions in environmental samples. The work reported shows the successful application of another mercury-free sensor electrode for the determination of platinum group metals in environmental samples. The work reported in this study entails the use of a glassy carbon electrode modified with a bismuth film for the determination of platinum (Pt(2+)), palladium (Pd(2+)) or rhodium (Rh(2+)) by means of adsorptive cathodic stripping voltammetry. Optimised experimental conditions included composition of the supporting electrolyte, complexing agent concentration, deposition potential, deposition time and instrumental voltammetry parameters for Pt(2+), Pd(2+) and Rh(2+) determination. Adsorptive differential pulse stripping voltammetric measurements for PGMs were performed in the presence of dimethylglyoxime (DMG) as complexing agent. The glassy carbon bismuth film electrode (GC/BiFE) employed in this study exhibit good and reproducible sensor characteristics. Application of GC/BiFE sensor exhibited well-defined peaks and highly linear behaviour for the stripping analysis of the PGMs in the concentration range between 0 and 3.5 μg/L. The detection limit of Pd, Pt and Rh was found to be 0.12 μg/L, 0.04 μg/L and 0.23 μg/L, respectively for the deposition times of 90 s (Pd) and 150 s (for both Pt and Rh). Good

Coenzyme Q-0 (CoQ-0) is the only Coenzyme Q lacking an isoprenoid group on the quinoid ring, a feature important for its physico-chemical properties. Here, the redox behavior of CoQ-0 in buffered and non-buffered aqueous media was examined. In buffered aqueous media CoQ-0 redox chemistry can be described by a 2-electron-2-proton redox scheme, characteristic for all benzoquinones. In non-buffered media the number of electrons involved in the electrode reaction of CoQ-0 is still 2; however, the number of protons involved varies between 0 and 2. This results in two additional voltammetric signals, attributed to 2-electrons-1H(+) and 2-electrons-0H(+) redox processes, in which mono- and di-anionic compounds of CoQ-0 are formed. In addition, CoQ-0 exhibits a complex chemistry in strong alkaline environment. The reaction of CoQ-0 and OH(-) anions generates several hydroxyl derivatives as products. Their structures were identified with HPLC/MS. The prevailing radical reaction mechanism was analyzed by electron paramagnetic resonance spectroscopy. The hydroxyl derivatives of CoQ-0 have a strong antioxidative potential and form stable complexes with Ca(2+) ions. In summary, our results allow mechanistic insights into the redox properties of CoQ-0 and its hydroxylated derivatives and provide hints on possible applications. PMID:27268099

Citrus limon peel (kitchen waste) and Leucaena leucocephala seeds (agricultural waste) were used as a modifier for fabrication of modified carbon paste electrode for determination of mercury in aqueous sample using differential pulse anodic stripping voltammetry. Mercury was adsorbed on electrode surface at open circuit and anodic stripping voltammetric scan was run from -0.5 to 0.5 V. Various electrochemical parameters including amount of modifier, supporting electrolyte, accumulating solvent, pH of the accumulating solvent, and accumulation time were investigated. The effect of presence of other metal ions and surfactants was also studied. In comparison C. limon peel proved to be a better modifier than L. leucocephala seed biomass. This was justified by electrode characterization using cyclic voltammetry that indicated decrease in resistance of electrode when C. limon peel was used as modifier and increase when modifier was L. leucocephala seeds. Maximum current response was obtained using 5% C. limon peel biomass, hydrochloric acid as supporting electrolyte, acetate buffer of pH 6 as an accumulating solvent, 10-min accumulation time, and scan rate of 50 mV/s. Linear calibration curves were obtained in the concentration range 100 to 1,000 μg L(-1) of mercury for accumulation time of 10 min with limit of detection of 57.75 μg L(-1) and limit of quantification of 192.48 μg L(-1). This technique does not use mercury as electrode material and, therefore, has a positive environmental benefit. PMID:23709264

A simple and reliable method for preparing a selective dopamine (DA) sensor based on a molecularly imprinted polymer of ethacridine was proposed. The molecularly imprinted polymer electrode was prepared through electrodepositing polyethacridine-dopamine film on the glassy carbon electrode and then removing DA from the film via chemical induced elution. The molecular imprinted sensor was tested by cyclic voltammetry as well as by differential pulse voltammetry (DPV) to verify the changes in oxidative currents of DA. In optimized DPV conditions the oxidation peak current was well-proportional to the concentration of DA in the range from 2.0×10(-8)M up to 1×10(-6)M. The limit of detection (3σ) of DA was found to be as low as 4.4nM, by the proposed sensor that could be considered a sensitive marker of DA depletion in Parkinson's disease. Good reproducibility with relative standard deviation of 1.4% and long term stability within two weeks were also observed. The modified sensor was validated for the analysis of DA in deproteinized human serum samples using differential pulse voltammetric technique. PMID:27591643

This study demonstrates the feasibility of using a voltammetric electronic tongue to monitor effluent dissolved orthophosphate concentration in a struvite precipitation reactor. The electrochemical response of the electronic tongue to the presence of orthophosphate in samples collected from the effluent of the precipitation reactor is used to predict orthophosphate concentration via a statistical model based on Partial Least Squares (PLS) Regression. PLS predictions were suitable for this monitoring application in which precipitation efficiencies higher than 80% (i.e., effluent dissolved orthophosphate concentrations lower than 40mg P-PO4(3-) L(-1)) could be considered as indicator of good process performance. The electronic tongue consisted of a set of metallic (noble and non-noble) electrodes housed inside a stainless steel cylinder which was used as the body of the electronic tongue system. Fouling problems were prevented via a simple mechanical polishing of the electrodes. The measurement of each sample with the electronic tongue was done in less than 3s. Conductivity of the samples only affected the electronic tongue marginally, being the main electrochemical response due to the orthophosphate concentration in the samples. Copper, silver, iridium and rhodium were the electrodes that exhibited noticeable response correlated with the dissolved orthophosphate concentration variations, while gold, platinum and especially cobalt and nickel were the less useful electrodes for this application. PMID:27474282

A highly sensitive and simple voltammetric method is proposed for the determination of N-nitrosoatenolol (NA) and N-nitrosopropranolol (NP) in simulated gastric juice. The method is based on measuring the differential-pulse polarographic peak produced by NA and NP in Britton-Robinson buffers of pH 3 and 4 for NA and NP, respectively. Both compounds yielded diffusion-controlled current with diffusion-current constants of 7.23 +/- 0.03 and 9.46 +/- 0.06 for NA and NP, respectively. The current-concentration plots were rectilinear over the range 0.16-9.6 micrograms ml-1 with minimum detectability (S/N = 2) of 0.015 microgram ml-1 (5 x 10(-8) M) for NA; for NP the range was 0.08-8.0 micrograms ml-1 with minimum detectability (S/N = 2) of 0.009 microgram ml-1 (3 x 10(-8) M). The proposed method was successfully applied to study the possible in vivo production of the nitroso-derivatives under the standard nitrosation reaction conditions recommended by WHO. The method is characterized by simplicity and higher sensitivity as compared with the reported HPLC method. PMID:10575740

A fullerene-C(60)-modified glassy carbon electrode (GCE) is used for the simultaneous determination of adenosine and guanosine by differential pulse voltammetry. Compared to a bare glassy carbon electrode, the modified electrode exhibits an apparent shift of the oxidation potentials in the cathodic direction and a marked enhancement in the voltammetric peak current response for both the biomolecules. Linear calibration curves are obtained over the concentration range 0.5muM-1.0mM in 0.1M phosphate buffer solution at pH 7.2 with a detection limit of 3.02x10(-7)M and 1.45x10(-7)M for individual determination of adenosine and guanosine, respectively. The interference studies showed that the fullerene-C(60)-modified glassy carbon electrode exhibited excellent selectivity in the presence of hypoxanthine, xanthine, uric acid and ascorbic acid. The proposed procedure was successfully applied to detect adenosine and guanosine in human blood plasma and urine, without any preliminary pre-treatment. PMID:19071420

Rhodium (Rh) is present at the Earth's surface at ultra-trace concentrations (0.06 ng g(-1)); however, its use in catalytic converters has increased its deposition nearby traffic pressure and therefore the interest in analytical techniques for Rh determination has raised in the recent years. In this study we propose an improvement of Rh measurement by adsorptive voltammetry applying second-derivative signal transformation. The optimization of experimental parameters affecting the voltammetric analysis were carried out using sediment samples; these include the amount of sample digest used, the hydrochloric acid and formaldehyde concentrations, deposition potential and equilibration time. The use of the second derivative transformation provided well-defined peaks due to the minimization of background interferences, leading to a significant decrease in the detection limits. Accordingly, a detection limit of 200 fM Rh in the cell was obtained, which corresponds to 14 pg g(-1) of Rh for 200mg of sediments. The optimized methodology was applied to the analysis of Rh in a sediment core collected close to a motorway bridge from Tagus Estuary (Lisbon, Portugal). Here, Rh concentrations ranged from 0.06 to 0.47 ng g(-1), showing a surface Rh-enrichment linked to traffic, which was consistent with a Pt superficial peak. Reference materials were also analyzed, including road dust (BCR-723) and river sediment (JSD-2), and values obtained were in agreement with certified concentrations and previously values reported in the literature. PMID:26695324

This work reported new voltammetric/amperometric-based protocols using a commercial boron-doped diamond (BDD) electrode for simple and fast simultaneous detection of sulfide and nitrite from water. Square-wave voltammetry operated under the optimized working conditions of 0.01 V step potential, 0.5 V modulation amplitude and 10 Hz frequency allowed achieving the best electroanalytical parameters for the simultaneous detection of nitrite and sulfide. For practical in-field detection applications, the multiple-pulsed amperometry technique was operated under optimized conditions, i.e., −0.5 V/SCE for a duration of 0.3 s as conditioning step, +0.85 V/SCE for a duration of 3 s that assure the sulfide oxidation and +1.25 V/SCE for a duration of 0.3 s, where the nitrite oxidation occurred, which allowed the simultaneously detection of sulfide and nitrite without interference between them. Good accuracy was found for this protocol in comparison with standardized methods for each anion. Also, no interference effect was found for the cation and anion species, which are common in the water matrix. PMID:26102487

Electrodeposition was used to prepare a new solid phase microextraction (SPME) coatings. Two apatite SPME coatings, dicalcium phosphate dihydrate (DCPD or brushite) and hydroxyapatite (HAP) were validly and homogeneously one-step electrodeposited on glassy carbon electrode (GCE) under different conditions. The coatings were characterized by XRD, FTIR, SEM, CV and EIS. The apatite SPME coatings showed excellent and selective adsorbability to fluoride ions. A novel indirect voltammetric strategy for sensitive detection of fluoride was proposed using K3Fe(CN)6 as indicating probe. The detection principle of fluoride ions was based on the increment of steric hindrance after fluoride adsorption, which resulting in the decrease of the amperometric signal to Fe(CN)6(3-). The liner ranges were 0.5-20.0 μmol/L for n-DCPD/GCE with the limit of detection of 0.14 μmol/L and 0.1-50.0 μmol/L for n-HAP/GCE with the limit of detection of 0.069 μmol/L, respectively. The developed method was applied to the analysis of water samples (lake, spring and tap water) and the recovery values were found to be in the range of 90-106%. PMID:24054624

A sensitive method for the measurement of phenazopyridine hydrochloride (PAP) by differential pulse polarography (DPP) based on adsorptive stripping technique, using a hanging mercury drop electrode (HMDE) is described. The voltammetric peak is obtained at -0.760 V, which corresponds to the reduction of the azo group in Britton-Robinson buffer. The redox behaviour is reversible. Optimum conditions were found to be: accumulation potential -50 mV (vs. Ag/AgCl), accumulation time 60 s, scan rate 5 mV s(-1), pulse amplitude -100 mV and supporting electrolyte Britton-Robinson buffer (0.04 M, pH=11). The relative standard deviation (at 20 ng ml(-1) level) was +/-0.6% for six measurements. The calculated detection limit was 0.0299 ng ml(-1) with a 60-s accumulation time. The applicability of such a method was evaluated through the assay of PAP in human plasma and urine samples after a simple extraction procedure and in pharmaceutical preparation. The mean recovery was 97+/-2 (100 ng ml(-1) plasma). PMID:18967703

In this study, the electrochemical behavior of eugenol, a widely used herbal drug, was investigated at a pencil graphite electrode (PGE). A low-cost, disposable, sensitive and selective electrochemical sensor is proposed for the determination of eugenol by recording its differential pulse voltammograms in Britton-Robinson buffer solution containing 0.1 M KCl with pH of 2.0 at the PGE. The PGE displayed a very good electrochemical behavior with significant enhancement of the peak current compared to a glassy carbon electrode. Under experimental conditions, the PGE had a linear response range from 0.3 μM to 50.0 μM eugenol with a detection limit of 0.085 μM (based on 3S(b)). Relative standard deviations of 2.4 and 4.8% were obtained for five successive determinations of 30.0 and 5.0 μM eugenol, respectively, which indicate acceptable repeatability. This voltammetric method was successfully applied for the direct determination of eugenol in real samples. The effect of various interfering compounds on the eugenol peak current was also studied. PMID:26706519

This paper describes a new method based on a voltammetric electronic tongue (ET) for the recognition of distinctive features in coffee samples. An ET was directly applied to different samples from the main Mexican coffee regions without any pretreatment before the analysis. The resulting electrochemical information was modeled with two different mathematical tools, namely Linear Discriminant Analysis (LDA) and Support Vector Machines (SVM). Growing conditions (i.e., organic or non-organic practices and altitude of crops) were considered for a first classification. LDA results showed an average discrimination rate of 88% ± 6.53% while SVM successfully accomplished an overall accuracy of 96.4% ± 3.50% for the same task. A second classification based on geographical origin of samples was carried out. Results showed an overall accuracy of 87.5% ± 7.79% for LDA and a superior performance of 97.5% ± 3.22% for SVM. Given the complexity of coffee samples, the high accuracy percentages achieved by ET coupled with SVM in both classification problems suggested a potential applicability of ET in the assessment of selected coffee features with a simpler and faster methodology along with a null sample pretreatment. In addition, the proposed method can be applied to authentication assessment while improving cost, time and accuracy of the general procedure. PMID:25254303

A novel and selective enzymatic biosensor was designed and constructed for voltammetric determination of levodopa (L-Dopa) in aqueous media (phosphate buffer solution, pH=7). Biosensor development was on the basis of to physically immobilizing of horse radish peroxidase (HRP) as electrochemical catalyst by sol-gel on glassy carbon electrode modified with organic nucleophilic carbon nanotube composite which in this composite p-phenylenediamine (pPDA) as organic nucleophile chemically bonded with functionalized MWCNT (MWCNT-COOH). The results of this study suggest that prepared bioorganic nucleophilic carbon nanotube composite (HRP/MWCNT-pPDA) shows fast electron transfer rate for electro oxidation of L-Dopa because of its high electrochemical catalytic activity toward the oxidation of L-Dopa, more--NH2 reactive sites and large effective surface area. Also in this work we measured L-Dopa in the presence of folic acid and uric acid as interferences. The proposed biosensor was characterized by scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), FT-IR spectroscopy and cyclic voltammetry (CV). The differential pulse voltammetry (DPV) was used for determination of L-Dopa from 0.1 μM to 1.9 μM with a low detection limit of 40 nM (for S/N=3) and sensitivity was about 35.5 μA/μM. Also this biosensor has several advantages such as rapid response, high stability and reproducibility. PMID:26478378

This work presents an approach to study the performance of novel targets able to overcome cancer stem cell chemoresistance, based on the voltammetric data for microparticulate films of natural or synthetic alkaloids from the canthin-6-one series. A comparison of this voltammetric technique with conventional solution phase electrochemistry suggests the differences in the anti-proliferative activity of canthin-6-ones could be tentatively correlated to their different capacity to generate semiquinone radical anions. These data also match theoretical calculations.

This paper presents an original integration of polycrystalline SiGe-based quantum dots superlattices (QDSL) into Thermoelectric (TE) planar infrared microsensors (μSIR) fabricated using a CMOS technology. The nanostructuration in QDSL results into a considerably reduced thermal conductivity by a factor up to 10 compared to the one of standard polysilicon layers that are usually used for IR sensor applications. A presentation of several TE layers, QDSL and polysilicon, is given before to describe the fabrication of the thermopile-based sensors. The theoretical values of the sensitivity to irradiance of μSIR can be predicted thanks to an analytical model. These findings are used to interpret the experimental measurements versus the nature of the TE layer exploited in the devices. The use of nanostructured QDSL as the main material in μSIR thermopile has brought a sensitivity improvement of about 28% consistent with theoretical predictions. The impact of QDSL low thermal conductivity is damped by the contribution of the thermal conductivity of all the other sub-layers that build up the device.

We report a temperature sensing system incorporated into an amperometric oxygen sensor. In the first part of this work, we introduce temperature sensing systems based upon voltammetric responses of both single molecule (1,2-diferrocenylethylene in 1-propyl-3-methylimidazolium bistrifluoromethylsulfonylimide) and two independent molecules (decamethylferrocene and N,N,N',N'-tetramethyl-p-phenylenediamine in 1-ethyl-3-methylimidazolium tetracyanoborate) respectively. In both systems, the difference in the formal potentials of two redox centres was measured as a function of temperature. The former was recorded as the peak difference in square wave voltammetry with the peak potential difference increases linearly with the increasing temperature. In order to show proof-of-concept in relation to a gas sensor, the latter system was investigated in the presence of oxygen, where the concentration and diffusion coefficient of oxygen varied with temperature, as well as the peak difference discussed previously, were studied in the presence of pure oxygen and dried air using chronoamperometry. A negligible variation of concentration of oxygen from both sources with temperature over the range 298 K to 318 K is demonstrated. These results obtained from pure oxygen and dried air were compared and a ca. 79% drop of cathodic signal from pure oxygen to dried air was found which is consistent with the percentage of oxygen in air. The diffusion coefficient of oxygen was related to temperature using an Arrhenius plot (natural log of diffusion coefficient as a function of reciprocal temperature), yielding a linear graph with high correlation. All experiments gave a high reproducibility. PMID:22534882

Square-wave adsorptive stripping voltammetric (SW-AdSV) determinations of trace concentrations of the coloring agent fast green were described. The analytical methodology used was based on the adsorptive preconcentration of the dye on the hanging mercury drop electrode, and then a negative sweep was initiated. In pH 10 carbonate supporting electrolyte, fast green gave a well-defined and sensitive SW-AdSV peak at -1220 mV. The electroanalytical determination of this dye was found to be optimized in carbonate buffer (pH 10) with the following experimental conditions: accumulation time (120 s); accumulation potential (-0.8 V); scan rate (800 mV/s); pulse amplitude (90 mV); frequency (90 Hz); surface area of the working electrode (0.6 mm2); and the convection rate (2000 rpm). Under these optimized conditions, the AdSV peak current was proportional over the concentration range 2 x 10(-8) -6 x 10(-7) M (r = 0.999), with an LOD of 1.63 x 10(-10) M (0.132 ppb). This analytical approach possessed more enhanced sensitivity than conventional chromatography or spectrophotometry, and was simple and quick. The precision of the method in terms of RSD was 0.17%, whereas the accuracy was evaluated via the mean recovery of 99.6%. Possible interferences by several substances usually present as food additive azo dyes (E110, E102, E123, and E129), natural and artificial sweeteners, and antioxidants were also investigated. Applicability of the developed electroanalysis method was illustrated via the determination of fast green in ice cream and soft drink samples. PMID:20166589

Aluminum is one of the abundant elements in the earth`s crust. It has been considered to be a causative agent for various neurological disorders such as Alzheimer Senile, presenile dementia and amyotrophic lateral sclerosis. It is also very harmful to plants and aquatic organisms. Therefore, the determination of Al is very important. A Pyrocatechol Violet (PCV) modified electrode for the voltammetric determination of aluminum is reported. The modified electrode is simply prepared by dip-coating a pyrolytic graphite electrode in a NaAc-HAc buffer solution of PCV. Optimum experimental conditions for aluminum determination include a 0.2 mol/L NaAc-HAc buffer solution of pH 4.8, a PCV concentration of 0.02 mol/L used to modify the electrode and the use of differential-pulse mode for measurement. The peak currents of differential pulse voltammograms (DPV) decrease with the addition of Al into the buffer solution while the peak potentials remain the same. The decreasing value of peak current {Delta}i{sub p} is linear with Al concentration in the range of 1{times}10{sup {minus}8} to 1{times}10{sup {minus}7} mol/L and 1{times}10{sup {minus}7} to 1{times}10{sup {minus}6} mol/L. The detection limit is 5{times}10{sup {minus}9} mol/L and the relative standard deviation for 4{times}10{sup {minus}8} mol/L Al is 2.9% (n=8). The stability of this electrode is satisfactory. No serious interference is found. This method has been applied to determine Al in drinking water samples.

A new electronic tongue to monitor the presence of glyphosate (a non-selective systemic herbicide) has been developed. It is based on pulse voltammetry and consists in an array of three working electrodes (Pt, Co and Cu) encapsulated on a methacrylate cylinder. The electrochemical response of the sensing array was characteristic of the presence of glyphosate in buffered water (phosphate buffer 0.1 mol·dm−3, pH 6.7). Rotating disc electrode (RDE) studies were carried out with Pt, Co and Cu electrodes in water at room temperature and at pH 6.7 using 0.1 mol·dm−3 of phosphate as a buffer. In the presence of glyphosate, the corrosion current of the Cu and Co electrodes increased significantly, probably due to the formation of Cu2+ or Co2+ complexes. The pulse array waveform for the voltammetric tongue was designed by taking into account some of the redox processes observed in the electrochemical studies. The PCA statistical analysis required four dimensions to explain 95% of variance. Moreover, a two-dimensional representation of the two principal components differentiated the water mixtures containing glyphosate. Furthermore, the PLS statistical analyses allowed the creation of a model to correlate the electrochemical response of the electrodes with glyphosate concentrations, even in the presence of potential interferents such as humic acids and Ca2+. The system offers a PLS prediction model for glyphosate detection with values of 098, −2.3 × 10−5 and 0.94 for the slope, the intercept and the regression coefficient, respectively, which is in agreement with the good fit between the predicted and measured concentrations. The results suggest the feasibility of this system to help develop electronic tongues for glyphosate detection. PMID:23250277

A simple and sensitive voltammetric method was developed to determine the amount of nitrite by using Carbon Paste Electrode (CPE) which is modified with polyvinylimidazole (PVI). A buffer solution of phosphate with a pH 4 value was used in the experiments. The amount of the nitrite-ion was determined by cyclic voltammetry (CV). The electro-chemical behaviour of nitrite-ion was investigated by using CV on the PVI modified CPE. A well-defined oxidation peak was obtained at 0.83 V against a reference Ag/AgCl electrode. Differential pulse voltammetry (DPV) was applied for the calibration plot and for the detection limit. The optimisation procedure was done in two steps: using a two-level factorial design for preliminary evaluation of the contributing factors, and the Box-Behnken Design (BBD) to assess the optimal experimental conditions. These are done with the analysis of 3 different factors in 15 runs of DPV. The optimum conditions are obtained within a linear response range of 5×10(-7)-1×10(-4) mol L(-1). Regression analysis is performed within this range showed the linear equation of y=0.028x+3.93×10(-7) with r(2)=0.9982, and for n=7. Limit of Detection (LOD) was 9×10(-8) mol L(-1) with S/N=3, and Limit of Quantification (LOQ) was 3×10(-7) mol L(-1) with S/N=10. The procedure was used successfully to detect the amount of nitrite in meat products. PMID:24444933

Background Lidocaine hydrochloride (LH) is one of the most extensively used local anesthetics and peripheral analgesics. Availability of a simple and sensitive assay method for this analyte in pharmaceutical preparations as well as development of new voltammetric detectors that can be applied in chromatographic systems for determination of this analyte in biological samples are of great importance. Objectives In this study, a square-wave voltammetric (SWV) determination of LH at a bare carbon-paste electrode (CPE) was reported. Moreover, the oxidation mechanism for LH molecule at this electrode was investigated. Materials and Methods The SW voltammogram of LH solution at CPE showed a well-defined peak between +0.80 and +0.88 V depending on a scan rate in potassium nitrate (KNO3) solution. Different chemical and instrumental parameters influencing the voltammetric response, such as the pH level and scan rate were optimized for LH determination. Results A linear range of 8.0 - 1000.0 μmol L-1 (r2 = 0.999) was obtained. The limit of detection (LOD) was 0.29 μmol L-1. The relative standard deviations of 2.1% obtained for 0.8 800 μmol L-1 solution of LH indicated a reasonable reproducibility of the method. Conclusions The results of this study show that LH in different pharmaceutical preparations could be determined with good reliability. In addition, the results reveal that the equal numbers of electrons and protons are involved in the oxidation of LH and the irreversible oxidation of an analyte was performed via amine groups of LH molecule. PMID:25866720

A new penicillamine-GCE was developed based on the immobilization of d-penicillamine on aryl diazonium salt monolayers anchored to the glassy carbon electrode (GCE) surface and it was applied for the first time to the simultaneous determination of Cd(II) and Pb(II) ions by stripping voltammetric techniques. The detection and quantification limits at levels of µg L(-1) suggest that the penicillamine-GCE could be fully suitable for the determination of the considered ions in natural samples. PMID:26452863

A novel microsensor, consisting of crossed Cu micropillars coated with ZnO nanorods, was fabricated by electrochemical methods for detecting gas in a small space. The Cu micropillars (80 μm diameter, 10 mm long) were prepared by microanode-guided electroplating (MAGE) on the periphery of a square copper pad (dimensions 5.0 mm × 5.0 mm × 1.0 mm). The micropillars were electrochemically coated with a 500 nm thick layer of ZnO nanorods deposited from a bath containing 2.0 mM zinc chloride and H2O2 varying in 5, 10, 15, and 20 mM. Two ZnO-coated pillars were crossed to form a microsensor by approaching the Cu pads below, which was adhered to an alumina substrate with silver paste and connected to conducting wires for measurement. The morphology of the coating of ZnO nanorods, which was found to be determined by the concentration of H2O2 in the bath, influenced the gas sensing. The morphology of the coating was characterized by scanning electron microscopy; the structural analysis was carried out by X-ray diffraction and high-resolution transmission electron microscopy (HRTEM); the surface analysis was carried out by X-ray photoelectron spectroscopy; and the defects were determined with photoluminescence (PL) spectra. We thus investigated the effect of the morphology of the coating on the sensing properties by introducing a stream of gases varying in CO/air ratios to understand the sensing mechanism of the microsensor. PMID:24960114

A simple and sensitive electroanalytical method was developed for determination of nanomolar levels of Pb(II) based on the voltammetric stripping response at a carbon paste electrode modified with biochar (a special charcoal) and bismuth nanostructures (nBi-BchCPE). The proposed methodology was based on spontaneous interactions between the highly functionalized biochar surface and Pb(II) ions followed by reduction of these ions into bismuth nanodots which promote an improvement on the stripping anodic current. The experimental procedure could be summarized in three steps: including an open circuit pre-concentration, reduction of accumulated lead ions at the electrode surface and stripping step under differential pulse voltammetric conditions (DPAdSV). SEM images revealed dimensions of bismuth nanodots ranging from 20 nm to 70 nm. The effects of main parameters related to biochar, bismuth and operational parameters were examined in detail. Under the optimal conditions, the proposed sensor has exhibited linear range from 5.0 to 1000 nmol L(-1) and detection limit of 1.41 nmol L(-1) for Pb(II). The optimized method was successfully applied for determination of Pb(II) released from overglaze-decorated ceramic dishes. Results obtained were compared with those given by inductively coupled plasma optical emission spectroscopy (ICP-OES) and they are in agreement at 99% of confidence level. PMID:26003715

Principal component regression, a multivariate calibration technique, is an invaluable tool for the analysis of voltammetric data collected in vivo with acutely implanted microelectrodes. This method utilizes training sets to separate cyclic voltammograms into contributions from multiple electroactive species. The introduction of chronically implanted microelectrodes permits longitudinal measurements at the same electrode and brain location over multiple recordings. The reliability of these measurements depends on a consistent calibration methodology. One published approach has been the use of training sets built with data from separate electrodes and animals to evaluate neurochemical signals in multiple subjects. Alternatively, responses to unpredicted rewards have been used to generate calibration data. This study addresses these approaches using voltammetric data from three different experiments in freely moving rats obtained with acutely implanted microelectrodes. The findings demonstrate critical issues arising from the misuse of principal component regression that result in significant underestimates of concentrations and improper statistical model validation that, in turn, can lead to inaccurate data interpretation. Therefore, the calibration methodology for chronically implanted microelectrodes needs to be revisited and improved before measurements can be considered reliable. PMID:26477708

A simple and selective thallium imprinted polymer was synthesized as a chemical modifier for the stripping voltammetric determination of Tl ions. The polymerization process (bulk polymerization) was performed with ethylene glycol dimethacrylate (crosslinking monomer) and methacrylic acid (functional monomer) in the presence of 2,2'-azobis(isobutyronitrile) (initiator). The electrochemical method was based on the accumulation of thallium ions at the surface of a modified carbon paste electrode with Tl imprinted polymer and multi-walled carbon nanotubes. After preconcentration process, the voltammetric measurements were carried out via electrolysis of the accumulated Tl ions in a closed circuit. Under the optimized conditions, a linear response range from 3.0 to 240 ng mL(-1) was obtained. The detection limit and RSD (100.0 ng mL(-1) of Tl) were calculated as 0.76 ng mL(-1) and ±2.7%, respectively. The suggested modified electrode has good characteristics such as excellent selectivity, high sensitivity and suitable stability. Also, it was successfully applied for the electrochemical determination of trace amounts of Tl in the environmental and biological samples. PMID:26452811

Low seawater pH can be harmful to many calcifying marine organisms, but the calcifying macroalgae Padina spp. flourish at natural submarine carbon dioxide seeps where seawater pH is low. We show that the microenvironment created by the rolled thallus margin of Padina australis facilitates supersaturation of CaCO3 and calcifi-cation via photosynthesis-induced elevated pH. Using microsensors to investigate oxygen and pH dynamics in the microenvironment of P. australis at a shallow CO2 seep, we found that, under saturating light, the pH inside the microenvironment (pHME ) was higher than the external seawater (pHSW ) at all pHSW levels investigated, and the difference (i.e., pHME - pHSW ) increased with decreasing pHSW (0.9 units at pHSW 7.0). Gross photosynthesis (Pg ) inside the microenvironment increased with decreasing pHSW , but algae from the control site reached a threshold at pH 6.5. Seep algae showed no pH threshold with respect to Pg within the pHSW range investigated. The external carbonic anhydrase (CA) inhibitor, acetazolamide, strongly inhibited Pg of P. australis at pHSW 8.2, but the effect was diminished under low pHSW (6.4-7.5), suggesting a greater dependence on membrane-bound CA for the dehydration of HCO3 (-) ions during dissolved inorganic carbon uptake at the higher pHSW . In comparison, a calcifying green alga, Halimeda cuneata f. digitata, was not inhibited by AZ, suggesting efficient bicarbonate transport. The ability of P. australis to elevate pHME at the site of calcification and its strong dependence on CA may explain why it can thrive at low pHSW . PMID:26987005

In situ chemical monitoring at deep-sea hydrothermal vents remains a challenge. Particularly, tools are still scarce for assessing the ranges and temporal variability of sulfide in these harsh environmental conditions. There is a particular need for compact and relatively simple devices to enlarge the capacity of in situ measurements of this major energy source in chemosynthetic ecosystems. With this objective, a voltammetric sensor based on a bare-silver working electrode was developed and tested in real conditions. In the laboratory, the sensor presented a linear response from 10 to 1000 μM sulfide, together with a low pH sensitivity and moderate temperature dependence. The device was operated at 850 and 2500 m depth during 3 cruises over two different vent fields. The autonomous potentiostat (290 mm length, ∅ 35 mm) equipped with laboratory-made electrodes was mounted on a wand, for manipulation from a submersible, or on a holder for unattended deployments. The system was applied in mussel, tubeworm and annelid worm habitats, characterized by different ranges of sulfide concentration, pH and temperature. Calibrations performed before and after each deployment confirmed the stability of the sensor response over a few hours to 11 days, with a maximum drift of 11.4% during this period. Short-term measurements in the vicinity of Riftia pachyptila and Alvinella pompejana were consistent with previous results on these habitats, with concentrations ranging from 20 to 140 μM and 100 to 450 μM and sulfide versus temperature ratio of 14 μM °C-1 and 20 μM °C-1, respectively. A continuous 4-day record on a bed of Bathymodiolus Thermophilus mussels furthermore illustrated the capacity of the sensor to capture fluctuating sulfide concentration between 0 and 70 μM, in combination to temperature, and to investigate the changes in the sulfide versus temperature ratio over time. The method has a higher detection limit (<10 μM) than previous in situ sulfide measurement

Four kinds of organic ion-selective microelectrodes (two barrels, tip diameter 0.1-0.5 micron) have been developed for the measurement of acetylcholine, histamine, serotonin, and bile acid. Physiological and pathological models on the cellular or sub-cellular level have been established for the purpose of basic and clinical pharmacological research, treatment or diagnosis of certain diseases. The acetylcholine sensitive microelectrode has been applied to the study of acetylcholine activity in single erythrocytes of normal human subjects and patients suffering from manic depressive disorders. The bile acid selective microelectrode has been used for the direct measurement of intracellular bile acid activities both in colorectal cancer and colorectal mucosa in living condition.

Stimuli-responsive hydrogels are materials with great potential for development of active functionalities in fluidics and micro-fluidics. Based on the current state of research on pH sensors, hydrogel sensors are described qualitatively and quantitatively for the first time. The review introduces the physical background of the special properties of stimuli-responsive hydrogels. Following, transducers are described which are able to convert the non-electrical changes of the physical properties of stimuli-responsive hydrogels into an electrical signal. Finally, the specific sensor properties, design rules and general conditions for sensor applications are discussed.

Herein is presented a microsensor technology as a diagnostic tool for detecting specific matrix metalloproteinases (MMPs) at very low concentrations. MMP-2 and MMP-9 are detected using label free porous silicon (PSi) photonic crystals that have been made selective for a given MMP by filling the nanopores with synthetic polymeric substrates containing a peptide sequence for that MMP. Proteolytic cleavage of the peptide sequence results in a shift in wavelength of the main peak in the reflectivity spectrum of the PSi device, which is dependent on the amount of MMP present. The ability to detect picogram amounts of MMP-2 and MMP-9 released by primary retinal pigment epithelial (RPE) cells and iris pigment epithelial (IPE) cells stimulated with lipopolysaccharide (LPS) is demonstrated. It was found that both cell types secrete higher amounts of MMP-2 than MMP-9 in their stimulated state, with RPE cells producing higher amounts of MMPs than IPE cells. The microsensor performance was compared to conventional protease detection systems, including gelatin zymography and enzyme linked immunosorbent assay (ELISA). It was found that the PSi microsensors were more sensitive than gelatin zymography; PSi microsensors detected the presence of both MMP-2 and MMP-9 while zymography could only detect MMP-2. The MMP-2 and MMP-9 quantification correlated well with the ELISA. This new method of detecting protease activity shows superior performance to conventional protease assays and has the potential for translation to high-throughput multiplexed analysis. PMID:26312479

The voltammetric performance of edge-plane pyrolytic graphite (EPG) electrode via adsorptive stripping voltammetry was investigated for study of the electrochemical behavior of omeprazole (OMZ) in aqueous solution. The results revealed that the oxidation of OMZ is an irreversible pH-dependent process that proceeds with the transfer of one electron and one proton in an adsorption-controlled mechanism. The determination conditions, such as the pH values of the supporting electrolyte, accumulation time and scan rate were optimized. Simplicity, high reproducibility and low detection limit (3 nM) of the electrode response as well as wide linear range (0.01 to 4.0 µM) can be stated as significant features of this electrode. The EPG electrode was successfully applied for the determination of OMZ in pharmaceutical formulations and satisfactory results were obtained. PMID:25901153

A hybrid electronic tongue based on data fusion of two different sensor families was built and used to recognize three types of beer. The employed sensor array was formed by three modified graphite-epoxy voltammetric sensors plus six potentiometric sensors with cross-sensitivity. The sensors array coupled with feature extraction and pattern recognition methods, namely Principal Component Analysis (PCA) and Discriminant Factor Analysis (DFA), were trained to classify the data clusters related to different beer types. PCA was used to visualize the different categories of taste profiles and DFA with leave-one-out cross validation approach permitted the qualitative classification. According to the DFA model, 96% of beer samples were correctly classified. The aim of this work is to prove performance of hybrid electronic tongue systems by exploiting the new approach of data fusion of different sensor families, in comparison of electronic tongue with only one sensor type.

The voltammetric performance of edge-plane pyrolytic graphite (EPG) electrode via adsorptive stripping voltammetry was investigated for study of the electrochemical behavior of omeprazole (OMZ) in aqueous solution. The results revealed that the oxidation of OMZ is an irreversible pH-dependent process that proceeds with the transfer of one electron and one proton in an adsorption-controlled mechanism. The determination conditions, such as the pH values of the supporting electrolyte, accumulation time and scan rate were optimized. Simplicity, high reproducibility and low detection limit (3 nM) of the electrode response as well as wide linear range (0.01 to 4.0 µM) can be stated as significant features of this electrode. The EPG electrode was successfully applied for the determination of OMZ in pharmaceutical formulations and satisfactory results were obtained. PMID:25901153

We report about testing a new mobile and sustainable water sample digestion method in a preliminary field trial in Ethiopia. In order to determine heavy metals at the ultra-trace level by stripping voltammetric techniques in water samples from Awash River, we applied our new method of solar UV-assisted sample pretreatment to destroy the relevant interfering dissolved organic matter. The field tests revealed that 24 h of solar UV irradiation were sufficient to achieve the same sample pretreatment results as with classic digestion method based on intense and hard UV. Analytical results of this study suggest that both a hydroelectric power station and agrichemical applications at Koka Lake have increased the levels of the investigated metals zinc, cadmium, lead, copper, cobalt, nickel, and uranium. PMID:27441266

This work reports the development of a glutathione modified electrode via electrografting on a screen-printed carbon nanofiber substrate (GSH-SPCNFE). GSH-SPCNFE was compared to a classical screen-printed carbon electrode modified with glutathione (GSH-SPCE) for the simultaneous voltammetric determination of Cd(II) and Pb(II). Their electrochemical characterization and analytical performance suggest that SPCNFE could be a much better support for GSH immobilization. The applicability of GSH-SPCNFE for the determination of low concentration levels of Pb(II) and Cd(II) ions in environmental samples was successfully tested in a certified wastewater reference material by means of stripping voltammetry with a very high reproducibility and good trueness. PMID:27216650

There has been an urgent need for an effective and efficient upper limb rehabilitation method for poststroke patients. We present a Micro-Sensor-based Upper Limb rehabilitation System for poststroke patients. The wearable motion capture units are attached to upper limb segments embedded in the fabric of garments. The body segment orientation relative to the reference frame is computed by fusion of the sensory data, and the upper limb trajectory and movement parameters are obtained. Using the micro-Sensor-based Upper Limb rehabilitation System, the clinical Active Range of Motion scale can be measured automatically; a set of novel quantitative measures, referred to as motor feature indices, are obtained to evaluate the quality of the movement. Experimental results show that the proposed motor feature indices reflect the real motor impairment status very well, providing objective measurements of a patient's functional recovery status in the rehabilitation process. PMID:22470053

Alternating current (ac) voltammetry provides access to faster electrode kinetics than direct current (dc) methods. However, difficulties in ac and other methods arise when the heterogeneous electron-transfer rate constant (k(0)) approaches the reversible limit, because the voltammetric characteristics become insensitive to electrode kinetics. Thus, in this near-reversible regime, even small uncertainties associated with bulk concentration (C), diffusion coefficient (D), electrode area (A), and uncompensated resistance (Ru) can lead to significant systematic error in the determination of k(0). In this study, we have introduced a kinetically sensitive dual-frequency designer waveform into the Fourier-transformed large-amplitude alternating current (FTAC) voltammetric method that is made up of two sine waves having the same amplitude but with different frequencies (e.g., 37 and 615 Hz) superimposed onto a dc ramp to quantify the close-to-reversible Fc(0/+) process (Fc = ferrocene) in two nonhaloaluminate ionic liquids. The concept is that from a single experiment the lower-frequency data set, collected on a time scale where the target process is reversible, can be used as an internal reference to calibrate A, D, C, and Ru. These calibrated values are then used to calculate k(0) from analysis of the harmonics of the higher-frequency data set, where the target process is quasi-reversible. With this approach, k(0) values of 0.28 and 0.11 cm·s(-1) have been obtained at a 50 μm diameter platinum microdisk electrode for the close-to-diffusion-controlled Fc(0/+) process in two ionic liquids, 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide and 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide, respectively. PMID:26771276

A sensitive glutamate biosensor is prepared based on glutamate dehydrogenase/vertically aligned carbon nanotubes (GLDH, VACNTs). Vertically aligned carbon nanotubes were grown on a silicon substrate by direct current plasma enhanced chemical vapor deposition (DC-PECVD) method. The electrochemical behavior of the synthesized VACNTs was investigated by cyclic voltammetry and electrochemical impedance spectroscopic methods. Glutamate dehydrogenase covalently attached on tip of VACNTs. The electrochemical performance of the electrode for detection of glutamate was investigated by cyclic and differential pulse voltammetry. Differential pulse voltammetric determinations of glutamate are performed in mediator-less condition and also, in the presence of 1 and 5 μM thionine as electron mediator. The linear calibration curve of the concentration of glutamate versus peak current is investigated in a wide range of 0.1-500 μM. The mediator-less biosensor has a low detection limit of 57 nM and two linear ranges of 0.1-20 μM with a sensitivity of 0.976 mA mM(-1) cm(-2) and 20-300 μM with a sensitivity of 0.182 mA mM(-1) cm(-2). In the presence of 1 μM thionine as an electron mediator, the prepared biosensor shows a low detection limit of 68 nM and two linear ranges of 0.1-20 with a calibration sensitivity of 1.17 mA mM(-1) cm(-2) and 20-500 μM with a sensitivity of 0.153 mA mM(-1) cm(-2). The effects of the other biological compounds on the voltammetric behavior of the prepared biosensor and its response stability are investigated. The results are demonstrated that the GLDH/VACNTs electrode even without electron mediator is a suitable basic electrode for detection of glutamate. PMID:22040749

Ultrasensitive ion-selective electrode measurements based on stripping voltammetry are an emerging sensor technology with low- and subnanomolar detection limits. Here, we report on stripping voltammetry of down to 0.1 nM Ca(2+) by using a thin-polymer-coated electrode and demonstrate the advantageous effects of the divalent charge on sensitivity. A simple theory predicts that the maximum concentration of an analyte ion preconcentrated in the thin membrane depends exponentially on the charge and that the current response based on exhaustive ion stripping from the thin membrane is proportional to the square of the charge. The theoretical predictions are quantitatively confirmed by using a thin ionophore-doped polymer membrane spin-coated on a conducting-polymer-modified electrode. The potentiostatic transfer of hydrophilic Ca(2+) from an aqueous sample into the hydrophobic double-polymer membrane is facilitated by an ionophore with high Ca(2+) affinity and selectivity. The resultant concentration of the Ca(2+)-ionophore complex in the ~1 μm-thick membrane can be at least 5 × 10(6) times higher than the aqueous Ca(2+) concentration. The stripping voltammetric current response to the divalent ion is enhanced to achieve a subnanomolar detection limit under the condition where a low-nanomolar detection limit is expected for a monovalent ion. Significantly, charge-dependent sensitivity is attractive for the ultrasensitive detection of multivalent ions with environmental and biomedical importance such as heavy metal ions and polyionic drugs. Importantly, this stripping voltammetric approach enables the absolute determination of subnanomolar Ca(2+) contamination in ultrapure water containing 10 mM supporting electrolytes, i.e., an 8 orders of magnitude higher background concentration. PMID:24992261

N'-(2-hydroxy-1,2-diphenylethylidene)benzohydrazide (HDB) was found to have a very selective and sensitive behavior towards erbium(III) ions, in comparison to thirteen lanthanide ions, inner transition and representative metal ions and was hence used as a neutral ion carrier in construction of an Er(III) microelectrode. Theoretical calculations and conductance studies of HDB to erbium and some other metal ions were carried out and confirmed selectivity toward Er(III) ions. The best performance was obtained with a membrane contain 3% potassium tetrakis(p-chlorophenyl)borate (KTpClPB) as an anionic additive, 72% dibutyl phthalate (DBP) as solvent mediator, 5% HDB, and 20% poly(vinyl chloride) (PVC). The proposed Er(III) microelectrode exhibits a near Nernstian response of 17.5±0.5 mV per decade of erbium activity, and a very wide linear range 1.0×10-3-3.0×10-10 M. It can work well in the pH range of 3.0-9.0. The lower detection limit (LDL) of the microelectrode was calculated to be 2.0×10-10 M.

The study presents an ammonia microsensor integrated with a readout circuit on-a-chip fabricated using the commercial 0.18 μm complementary metal oxide semiconductor (CMOS) process. The integrated sensor chip consists of a heater, an ammonia sensor and a readout circuit. The ammonia sensor is constructed by a sensitive film and the interdigitated electrodes. The sensitive film is zirconium dioxide that is coated on the interdigitated electrodes. The heater is used to provide a working temperature to the sensitive film. A post-process is employed to remove the sacrificial layer and to coat zirconium dioxide on the sensor. When the sensitive film adsorbs or desorbs ammonia gas, the sensor produces a change in resistance. The readout circuit converts the resistance variation of the sensor into the output voltage. The experiments show that the integrated ammonia sensor has a sensitivity of 4.1 mV/ppm. PMID:23503294

The voltammetric response of Au and Pt microdisk electrodes (6.4, 12.5, and 25 micrometers) in concentrated solutions of organic redox species (nitrobenzene, acetophenone and benzophenone) has been measured as a function of the orientation and magnitude of an externally applied magnetic field (0 - 1 Tesla). A magnetic field effect on voltammetric currents is observed for redox concentrations greater than approx. 0.01 M, and is a strong function of the orientation of the field. Large enhancements (+100%) or diminishments ({minus}15%) of limiting currents can be induced by application of the magnetic field. The observed phenomena are discussed in terms of magnetic field-induced transport of electrogenerated products.

ZnO-CuO nanoplates and 2-chlorobenzoyl ferrocene, were synthesized and used to construct a modified carbon paste electrode. The electrooxidation of 6-thioguanine at the surface of the modified electrode was studied. Under the optimized conditions, the square wave voltammetric (SWV) peak current of 6-thioguanine increased linearly in the concentration range 0.05 to 200.0μM and detection limit of 25±2nM was obtained for 6-thioguanine. The prepared modified electrode exhibits a very good resolution between the voltammetric peaks of 6-thioguanine and folic acid which makes it suitable for the detection of 6-thioguanine in the presence of folic acid in real samples. PMID:27612697

Ag-ZnO nanoplates and 2-chlorobenzoyl ferrocene were synthesized and used to construct a modified carbon paste electrode. The electrooxidation of glutathione at the surface of the modified electrode was studied. Under the optimized conditions, the square wave voltammetric (SWV) peak current of glutathione increased linearly with glutathione concentrations in the range of 5.0 × 10(-8) to 2.0 × 10(-4)M with sensitivity of 0.659 μA μM(-1) and method detection limit of 20.0 nM was obtained for glutathione. The prepared modified electrode exhibits a very good resolution between the voltammetric peaks of glutathione and tryptophan which makes it suitable for the detection of glutathione in the presence of tryptophan in real samples. PMID:26354245

This paper presents a high-Q resonant pressure microsensor with through-glass electrical interconnections based on wafer-level MEMS vacuum packaging. An approach to maintaining high-vacuum conditions by integrating the MEMS fabrication process with getter material preparation is presented in this paper. In this device, the pressure under measurement causes a deflection of a pressure-sensitive silicon square diaphragm, which is further translated to stress build up in “H” type doubly-clamped micro resonant beams, leading to a resonance frequency shift. The device geometries were optimized using FEM simulation and a 4-inch SOI wafer was used for device fabrication, which required only three photolithographic steps. In the device fabrication, a non-evaporable metal thin film as the getter material was sputtered on a Pyrex 7740 glass wafer, which was then anodically bonded to the patterned SOI wafer for vacuum packaging. Through-glass via holes predefined in the glass wafer functioned as the electrical interconnections between the patterned SOI wafer and the surrounding electrical components. Experimental results recorded that the Q-factor of the resonant beam was beyond 22,000, with a differential sensitivity of 89.86 Hz/kPa, a device resolution of 10 Pa and a nonlinearity of 0.02% F.S with the pressure varying from 50 kPa to 100 kPa. In addition, the temperature drift coefficient was less than −0.01% F.S/°C in the range of −40 °C to 70 °C, the long-term stability error was quantified as 0.01% F.S over a 5-month period and the accuracy of the microsensor was better than 0.01% F.S. PMID:25521385

Electrochemical measurements using voltammetry or amperometry at carbon-fiber microelectrodes have been used in vitro and in vivo to examine regulatory mechanisms for the central dopamine system. In many of these experiments, dopamine efflux concentrations under control conditions are determined followed by their alterations in response to a drug treatment. The present study demonstrates that some drugs can affect dopamine measurements, not only by their expected pharmacological action but also by directly altering the microelectrode responsivity. The commonly used reuptake inhibitors GBR 12909 (10 microM) and nomifensine (5 microM) drastically reduce electrode sensitivity and, in the case of nomifensine, increase the time to reach a plateau in response to dopamine boluses (i.e. reduced 'frequency response'). Cocaine (10 microM) and WIN 35428 (2 microM) have negligible effect on these indices. This decrease in sensitivity was found in both nafion and non-nafion coated electrodes. Further, the reduction in sensitivity seen in non-nafion coated electrodes was not prevented by increasing the reversal potential (from +1.0 to +1.3 V) and voltage scan rate (from 350 to 450 V/s). These data suggest that care must be taken when interpreting data from voltammetric or amporometric experiments using carbon electrodes where GBR 12909 or nomifensine are used, especially at high concentrations. Furthermore, wherever possible, direct effects of a drug on electrode sensitivity and frequency response should be determined. PMID:10967364

This paper presents a sensitive, selective and low-cost voltammetric method for the determination of caffeine using a Nafion covered lead film electrode. The sensor was prepared on a glassy carbon electrode modified with lead film recovered by a Nafion layer. Caffeine was accumulated and then oxidised at the modified electrode surface to produce two anodic peaks at 0.86 and 1.40 V (vs. Ag/AgCl) in 0.1 mol L(-1) H2SO4 medium. The obtained detection limits for caffeine following 120 s of accumulation time were equal to 1.7 × 10(-8) mol L(-1) (for peak 1) and 2.2 × 10(-7) mol L(-1) (for peak 2). The method was successfully applied to determination of caffeine in tea, coffee, soft and energy drink samples as well as pharmaceutical formulation and the contents closely corresponded to those quoted by the manufacturer and those obtained by the reported spectrophotometric method. PMID:25442519

In this work, a batch-injection analysis system with square-wave voltammetric (BIA-SWV) detection was applied for the first time to the simultaneous determination of inorganic (zinc) and organic (naphazoline) species. Both compounds were detected in a single run (70 injections h(-1)) with a small injection volume (∼100µL). The calibration curves exhibited linear response range between 3.0 and 21.0μmolL(-1) (r=0.999) for naphazoline and between 10.0 and 60.0μmolL(-1) (r=0.992) for zinc. The detection limits were 0.13 and 0.04μmolL(-1) for zinc and naphazoline, respectively. Good reproducibility was achieved for multiple measurements of a solution containing both species (RSD<1.0%; n=20). The results obtained with the BIA-SWV method for the simultaneous determination of naphazoline and zinc were compared to those obtained by HPLC (naphazoline) and by FAAS (zinc); no statistically significant differences were observed (95% confidence level). PMID:26992525

A new transfer mechanism is considered in which two different ionic species of the same charge can be transferred across a soft interface while they interconvert with each other in the original phase through a homogeneous chemical reaction: the aqueous complexation-dissociation coupled to transfer (ACDT) mechanism. This can correspond to a free ion in aqueous solution in the presence of a neutral ligand that complexes it leading to a species that can be more or less lipophilic than the free ion. As a result, the transfer to the organic phase can be facilitated or hindered by the aqueous-phase chemical reaction. Rigorous and approximate explicit analytical solutions are derived for the study of the above mechanism via normal pulse voltammetry, derivative voltammetry and chronoamperometry at macrointerfaces. The solutions enable us to examine the process whatever the species' lipophilicity and diffusivity in each medium and the kinetics and thermodynamics of the chemical reaction in solution. Moreover, when the chemical reaction is at equilibrium, explicit expressions for cyclic voltammetry and square wave voltammetry are obtained. With this set of equations, the influence of different physicochemical phenomena on the voltammetric response is studied as well as the most suitable strategies to characterize them. PMID:27020610

Essential oil of Carum copticum seeds, obtained from a local shop, was extracted and content of thymol was analyzed using square-wave voltammetry at boron-doped diamond electrode. The effect of various parameters, such as pH of supporting electrolyte and square-wave voltammetric parameters (modulation amplitude and frequency), was examined. In Britton-Robinson buffer solution (pH 4), thymol provided a single and oval-shaped irreversible oxidation peak at +1.13 V versus silver/silver chloride potassium electrode (3M). Under optimal experimental conditions, a plot of peak height against concentration of thymol was found to be linear over the range of 4 to 100μM consisting of two linear ranges: from 4 to 20μM (R(2)=0.9964) and from 20 to 100μM (R(2)=0.9993). The effect of potential interferences such as p-cymene and γ-terpinene (major components in essential oil of C. copticum seeds) was evaluated. Thus, the proposed method displays a sufficient selectivity toward thymol with a detection limit of 3.9μM, and it was successfully applied for the determination of thymol in essential oil of C. copticum seeds. The Prussian blue method was used for validation of the proposed electroanalytical method. PMID:26119334

A simple and highly selective electrochemical method was developed for the simultaneous determination of aspartame and cyclamate in dietary products at a boron-doped diamond (BDD) electrode. In square-wave voltammetric (SWV) measurements, the BDD electrode was able to separate the oxidation peak potentials of aspartame and cyclamate present in binary mixtures by about 400 mV. The detection limit for aspartame in the presence of 3.0x10(-4) mol L(-1) cyclamate was 4.7x10(-7) mol L(-1), and the detection limit for cyclamate in the presence of 1.0x10(-4) mol L(-1) aspartame was 4.2x10(-6) mol L(-1). When simultaneously changing the concentration of both aspartame and cyclamate in a 0.5 mol L(-1) sulfuric acid solution, the corresponding detection limits were 3.5x10(-7) and 4.5x10(-6) mol L(-1), respectively. The relative standard deviation (R.S.D.) obtained was 1.3% for the 1.0x10(-4) mol L(-1) aspartame solution (n=5) and 1.1% for the 3.0x10(-3) mol L(-1) cyclamate solution. The proposed method was successfully applied in the determination of aspartame in several dietary products with results similar to those obtained using an HPLC method at 95% confidence level. PMID:18585340

In this study, we reported iminodiacetic acid-copper ion complex (IDA-Cu) immobilized onto gold nanoparticles (GNPs)-modified glassy carbon electrode as a novel electrochemical platform for selective and sensitive determination of lysozyme (Lys). IDA-Cu complex acted as an efficient recognition element capable of capturing Lys molecules. GNPs acts as a substrate to immobilize IDA-Cu coordinative complex and its interaction with Lys leds to a great signal amplification through measuring changes in differential pulse voltammetric (DPV) peak current of [Fe(CN)6](3-/4-) redox probe. Upon the recognition of the Lys to the IDA-Cu, the peak current decreased due to the hindered electron transfer reaction on the electrode surface. Under optimum condition, it was found that the proposed method could detect Lys at wide linear concentration range (0.1 pM to 0.10 mM) with detection limit of 60 fM. Furthermore, electrochemical impedance spectroscopy (EIS) detection of Lys was demonstrated as a simple and rapid alternative analytical technique with detection limit of 80 fM at concentration range up to 0.1mM. In addition, the proposed sensor was satisfactorily applied to the determination of Lys in real samples such as hen egg white. The proposed modified electrode showing the high selectivity, good sensitivity and stability toward Lys detection may hold a great promise in developing other electrochemical sensors based on metal-chelate affinity complexes. PMID:26143467

The use of fast scan cyclic voltammetry (FSCV) to measure the release and uptake of dopamine (DA) as well as other biogenic molecules in viable brain tissue slices has gained popularity over the last 2 decades. Brain slices have the advantage of maintaining the functional three-dimensional architecture of the neuronal network while also allowing researchers to obtain multiple sets of measurements from a single animal. In this work, we describe a simple, easy-to-fabricate perfusion device designed to focally deliver pharmacological agents to brain slices. The device incorporates a microfluidic channel that runs under the perfusion bath and a microcapillary that supplies fluid from this channel up to the slice. We measured electrically evoked DA release in brain slices before and after the administration of two dopaminergic stimulants, cocaine and GBR-12909. Measurements were collected at two locations, one directly over and the other 500 μm away from the capillary opening. Using this approach, the controlled delivery of drugs to a confined region of the brain slice and the application of this chamber to FSCV measurements, were demonstrated. Moreover, the consumption of drugs was reduced to tens of microliters, which is thousands of times less than traditional perfusion methods. We expect that this simply fabricated device will be useful in providing spatially resolved delivery of drugs with minimum consumption for voltammetric and electrophysiological studies of a variety of biological tissues both in vitro and ex vivo. PMID:24734992

This work describes the development of a low-cost and reliable adsorptive stripping voltammetric method for the detection of PNP in water. Organoclays were prepared by intercalation in various loading amounts of cetyltrimethylammonium ions (CTA(+)) in the interlayer space of a smectite-type clay mineral. Their structural characterization was achieved using several techniques including X-ray diffraction (XRD), N2 adsorption-desorption (BET method) and Fourier Transform Infrared spectroscopy (FTIR) that confirmed the intercalation process and the presence of the surfactant ions within the clay mineral layers. Using [Fe(CN)6](3-) and [Ru(NH3)6](3+) as redox probes, the surface charge and the permeability of the starting clay mineral and its modified counterparts were assessed by multisweep cyclic voltammetry, when these materials were coated on the surface of a glassy carbon electrode (GCE). In comparison with the bare GCE, the organoclay modified electrodes exhibited more sensitive response towards the reduction of paranitrophenol (PNP). Under optimized conditions, a calibration curve was obtained in the concentration range from 0.2 to 5.2µmolL(-1); leading to a detection limit of 3.75×10(-8)molL(-1) (S/N=3). After the study of some interfering species on the electrochemical response of PNP, the developed sensor was successfully applied to the electroanalytical quantification of the same pollutant in spring water. PMID:26592645

Multi-walled carbon nanotube (MWCNTS) coated with poly p-aminobenzene sulfonic acid/β-cyclodextrin (p-ABSA/β-CD) film was used as an effective strategy for modification of the surface of glassy carbon electrode (GCE). Electrochemical study and determination of citalopram (CT) were investigated at the p (p-ABSA)/β-CD/MWCNT/GC using cyclic and differential pulse anodic stripping voltammetric techniques. The results indicate that the p (p-ABSA)/β-CD/MWCNT/GC significantly enhanced the oxidation peak current of CT. The modified electrode was characterized by electrochemical impedance spectroscopy (EIS), scanning electron microscopy(SEM) and cyclic voltammetry (CV).The fabricated electrochemical sensor exhibits a fast and reversible linear response toward CT within the concentration ranges of 90 nM-1 μM, 1-11 μM and 11-100 μM with correlation coefficients greater than 0.99 and detection limit of 44 nM. The resulting functionalized polymer film features interesting electrochemical properties such good recovery, reproducibility and selectivity toward CT. The applicability of the proposed sensor was tested by determination of CT in pharmaceutical combinations and human body fluids. PMID:26952450

Previous in situ voltammetric microelectrode measurements of median eminence dopamine release during mammary nerve stimulation of anesthetized lactating rats revealed a transient (1-3 min) 70% decline of dopamine concentrations. This dopamine was believed to be destined for secretion into the hypophysial portal circulation, but direct experimental support for this supposition was lacking. Thus, in the present study, (3H)dopamine release into brief sequential samples of hypophysial portal blood was compared with dopamine release in the median eminence measured by voltammetry. Lactating female rats were urethane anesthetized, and the median eminence pituitary region was exposed. (3H)Tyrosine was injected into a jugular cannula (100 microCi) followed by continuous infusion (5 microCi/min). In a preliminary experiment, this regimen produced a steady state level of (3H)dopamine in the portal blood within 45 min. In subsequent experiments, portal blood was collected as sequential 3-min samples, and electrochemical sampling from a microelectrode placed in the median eminence occurred at 1-min intervals. Electrochemical current resulting from the oxidation of dopamine in the medial median eminence was unvarying throughout the 75-min experiment in control rats (n . 4) and during the 30-min control period preceding mammary nerve stimulation in the other group (n . 4). These results were paralled by (3H) dopamine levels in portal blood during the same periods of time. All animals showed simultaneous decreases in oxidation current and (3H)dopamine levels within 1-4 min after initiation of mammary nerve stimulation. These and earlier results demonstrate that mammary nerve stimulation (and by extension, suckling) induces a momentary, but profound, decrease in hypothalamic dopamine secretion which precedes or accompanies the rise in PRL secretion evoked by the same stimulus.

Square-wave adsorptive stripping voltammetric (AdSV) determinations of trace concentrations of the azo coloring agent Amaranth are described. The analytical methodology used was based on the adsorptive preconcentration of the dye on the hanging mercury drop electrode, followed by initiation of a negative sweep. In a pH 10 carbonate supporting electrolyte, Amaranth gave a well-defined and sensitive AdSV peak at -518 mV. The electroanalytical determination of this azo dye was found to be optimal in carbonate buffer (pH 10) under the following experimental conditions: accumulation time, 120 s; accumulation potential, 0.0 V; scan rate, 600 mV/s; pulse amplitude, 90 mV; and frequency, 50 Hz. Under these optimized conditions the AdSV peak current was proportional over the concentration range 1 x 10(-8)-1.1 x 10(-7) mol/L (r = 0.999) with a detection limit of 1.7 x 10(-9) mol/L (1.03 ppb). This analytical approach possessed enhanced sensitivity, compared with conventional liquid chromatography or spectrophotometry and it was simple and fast. The precision of the method, expressed as the relative standard deviation, was 0.23%, whereas the accuracy, expressed as the mean recovery, was 104%. Possible interferences by several substances usually present as food additive azo dyes (E110, E102), gelatin, natural and artificial sweeteners, preservatives, and antioxidants were also investigated. The developed electroanalyticals method was applied to the determination of Amaranth in soft drink samples, and the results were compared with those obtained by a reference spectrophotometric method. Statistical analysis (paired t-test) of these data showed that the results of the 2 methods compared favorably. PMID:16001853

The electrochemical behavior of the anthelmintic veterinary drug nitroxynil at the mercury electrode was studied in a series of Britton-Robinson universal buffer of pH 1.9-11 containing 20% (v/v) ethanol using dc-polarography cyclic voltammetry and controlled-potential coulometry. The voltammograms exhibited two irreversible cathodic steps over the pH range 1.9-10.2; the height of the first step is double that of the second one. Controlled-potential coulometry in the B-R universal buffer of pH 1.9-10 at a mercury pool working electrode revealed the consumption of four and two electrons via the first and second reduction steps, respectively, which attributed to reduction of the NO2 group to the hydroxylamine stage (first step), and then to the amine stage (second step). Three voltammetric analytical procedures including dc-polarography, differential-pulse adsorptive stripping voltammetry and square-wave adsorptive stripping voltammetry were optimized for the direct determination of bulk nitroxynil. The three proposed procedures were applied for analysis of bulk nitroxynil with limits of detection of 3 x 10(-5), 1.31 x 10(-8) and 8.4 x 10(-10)M and limits of quantification of 1 x 10(-5), 4.36 x 10(-8) and 2.80 x 10(-9)M, respectively. The three procedures were successfully applied to the determination of nitroxynil in formulation (Dovenix, 25% nitroxynil injection solution) without the necessity for sample pretreatment and/or time-consuming extraction steps prior to the analysis. PMID:16687232

Nanoporous carbons, with different micropore size distributions, were prepared based on waste coffee grounds by a chemical activation process in order to elucidate the correlation between desolvated ions and pores smaller than the sizes of ions using an organic electrolyte. The pore structure of the coffee-based nanoporous carbon was strongly dependent on the heat-treatment temperature prior to the activation process. Cyclic voltammograms of the nanoporous carbons mainly dominated by the smaller pore relative to that of the bare ion size clearly showed deviation from an ideal feature of the current response. It was clearly envisaged that even a bare ion of a size larger than the pore size can penetrate into the pore by voltage-induced force. PMID:25668782

7,12-Dimethylbenz[a]anthracene (DMBA), is a widely studied polycyclic aromatic hydrocarbon that has long been recognized as a very potent carcinogen. Initially, the electrochemical oxidation of DMBA at the glassy carbon and pencil graphite electrodes in non-aqueous media (dimethylsulphoxide with lithium perchlorate) was studied by cyclic voltammetry. DMBA was irreversibly oxidized in two steps at high positive potentials, resulting in the ill-resolved formation of a couple with a reduction and re-oxidation wave at much lower potentials. Special attention was given to the use of adsorptive stripping voltammetry together with a medium exchange procedure on disposable pencil graphite electrode in aqueous solutions over the pH range of 3.0-9.0. The response was characterized with respect to pH of the supporting electrolyte, pre-concentration time and accumulation potential. Using square-wave stripping mode, the compound yielded a well-defined voltammetric response in acetate buffer, pH 4.8 at +1.15V (vs. Ag/AgCl) (a pre-concentration step being carried out at a fixed potential of +0.60V for 360s). The process could be used to determine DMBA concentrations in the range 2-10nM, with an extremely low detection limit of 0.194nM (49.7ngL(-1)). The applicability to assay of spiked human urine samples was also illustrated. Finally, the interaction of DMBA with fish sperm double-stranded DNA based on decreasing of the oxidation signal of adenine base was studied electrochemically by using differential pulse voltammetry with a pencil graphite electrode at the surface and also in solution. The favorable signal-to-noise characteristics of biosensor resulted in low detection limit (ca. 46nM) following a 300-s interaction. These results displayed that the electrochemical DNA-based biosensor could be used for the sensitive, rapid, simple and cost effective detection of DMBA-DNA interaction. PMID:20006098

Melatonin can be sensitively detected in pharmaceuticals by cyclic voltammetry and fixed-potential amperometry using a graphene-based sensor. The sensor characterization of cyclic voltammetry constantly provides high values of electrode active area and heterogeneous rate constant. In optimal conditions, the sensor was applied for the determination of melatonin in different pharmaceutical samples. The sensitivity to melatonin was 0.0371 A M−1, and the limit of detection was 0.87×10−6 M. The data obtained by using the graphene-based sensor for the detection of melatonin in pharmaceutical products were in good agreement with the data provided by the producer. Since no interferences from the excipients were found, using a separation technique was not necessary. Additionally, the low price, ease of handling, small amount of sample, short time per analysis, and possibility of automation are the important advantages that recommend this methodology for quality control of pharmaceuticals. PMID:27194909

Melatonin can be sensitively detected in pharmaceuticals by cyclic voltammetry and fixed-potential amperometry using a graphene-based sensor. The sensor characterization of cyclic voltammetry constantly provides high values of electrode active area and heterogeneous rate constant. In optimal conditions, the sensor was applied for the determination of melatonin in different pharmaceutical samples. The sensitivity to melatonin was 0.0371 A M(-1), and the limit of detection was 0.87×10(-6) M. The data obtained by using the graphene-based sensor for the detection of melatonin in pharmaceutical products were in good agreement with the data provided by the producer. Since no interferences from the excipients were found, using a separation technique was not necessary. Additionally, the low price, ease of handling, small amount of sample, short time per analysis, and possibility of automation are the important advantages that recommend this methodology for quality control of pharmaceuticals. PMID:27194909

In this work, graphene oxide was reduced to graphene with an endogenous reducing agent from dimethylformamide, and then AuPd alloy nanoparticles were electrodeposited on the graphene film. The obtained AuPd-graphene hybrid film was characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction and voltammetry. The electrochemical behavior of vanillin was studied using the AuPd-graphene hybrid based electrode. It presented high electrocatalytic activity and vanillin could produce a sensitive oxidation peak at it. Under the optimal conditions, the peak current was linear to the concentration of vanillin in the ranges of 0.1-7 and 10-40 μM. The sensitivities were 1.60 and 0.170 mA mM(-1) cm(-2), respectively; the detection limit was 20 nM. The electrode was successfully applied to the detection of vanillin in vanilla bean, vanilla tea and biscuit samples. PMID:24423501

This work reports the preparation of a voltammetric sensor for selective recognition and sensitive determination of mercury ions using a carbon ionic liquid paste electrode (CILE) impregnated with novel Hg(2+)-ion imprinted polymeric nanobeads (IIP) based on dithizone, as a suitable ligand for complex formation with Hg(2+) ions. The differential pulse anodic stripping voltammetric technique was employed to investigate the performance of the prepared IIP-CILE for determination of hazardous mercury ions. The designed modified electrode revealed linear responses in the ranges of 0.5nM-10nM and 0.08μM-2μM with a limit of detection of 0.1nM (S/N=3). It was found that the peak currents of the modified electrode for Hg(2+) ions were at a maximum value in phosphate buffer of pH4.5. The optimized preconcentration potential and accumulation time were to be -0.9V and 35s, respectively. The applicability of the proposed sensor to mercury determination in waste water samples is reported. PMID:25579915

A sequential injection analysis (SIA) system was developed with the aim of obtaining an automatic and versatile way to prepare standards needed in the study of systems with higher dimensional sensor signals. To illustrate this, different analytical techniques were used in determinations of several analytes. Automated potentiometric calibrations of different potentiometric sensors, with and without interference, were carried out. Useful determinations of selectivity coefficients with two degrees of freedom were obtained. Simultaneous voltammetric determinations have also been done. Firstly, simultaneous determinations of lead and cadmium, using epoxy-graphite composite as the working electrode, have enabled a separate calibration for each metal to be obtained. Next, a voltammetric electronic tongue was designed and applied to the determination of oxidizable species. The use of artificial neural networks has solved the overlapped signal of ascorbic acid, 4-aminophenol and 4-acetamidophenol (paracetamol). A set of 63 data points was prepared automatically and has facilitated the training of an electronic tongue for these three analytes. Accurate predictions of test solutions, in the range of 12-410muM for ascorbic acid, 17-530muM for 4-aminophenol and 10-420muM for paracetamol, have been achieved with RMSEs lower than 0.10muM. PMID:18970108

A novel voltammetric sensor was constructed by simple dripping single-walled carbon nanotubes (SWCNTs) on to the glass carbon electrode (GCE) firstly and electro-polymerizing L-Citrulline film subsequently. The resulting poly(L-Citrulline)/SWCNTs/GCE showed a significant voltammetric response to picroside II due to the synergistic effect of SWCNTs and poly(L-Citrulline) film. The first electroanalytical method of picroside II was proposed with detection linear range from 8.0 × 10(-8) to 5.0 × 10(-6) mol L(-1) and a detection limit of 3 × 10(-8) mol L(-1). The high sensitivity, selectivity and long-term stability made the sensor suitable for the determination of picroside II. Moreover, based on the systematically investigation and some kinetics parameters calculated in the experimentation, the reaction mechanism of picroside II at the poly(L-Citrulline)/SWCNTs modified GCE was obtained reliably. Lastly, the proposed sensor was used for the determination of picroside II in real sample with satisfactory results. This work promoted the potential applications of amino acid materials and SWCNTs in electro-chemical sensors. PMID:26838418

An Au nanoparticles/poly(caffeic acid) (AuNPs/PCA) composite modified glassy carbon (GC) electrode was prepared by successively potentiostatic technique in pH 7.4 phosphate buffer solution containing 0.02mM caffeic acid and 1.0mM HAuCl4. Electrochemical characterization of the AuNPs/PCA-GC electrode was investigated by electrochemical impedance spectroscopy and cyclic voltammetry. The electrochemical behavior of acetaminophen (AP) at the AuNPs/PCA-GC electrode was also studied by cyclic voltammetry. Compared with bare GC and poly(caffeic acid) modified GC electrode, the AuNPs/PCA-GC electrode was exhibited excellent electrocatalytic activity toward the oxidation of AP. The plot of catalytic current versus AP concentration showed two linear segments in the concentration ranges 0.2-20µM and 50-1000µM. The detection limit of 14 nM was obtained by using the first range of the calibration plot. The AuNPs/PCA-GC electrode has been successfully applied and validated by analyzing AP in blood, urine and pharmaceutical samples. PMID:27474318

This paper reports the fabrication of an insertable amperometric dual microsensor and its application for the simultaneous and fast sensing of NO and CO during acutely induced seizures of living rat brain cortex. NO and CO are important signaling mediators, controlling cerebrovascular tone. The dual NO/CO sensor is prepared based on a dual microelectrode having Au-deposited Pt microdisk (WE1, 76 μm diameter) and Pt black-deposited Pt disk (WE2, 50 μm diameter). The different deposited metals for WE1 and WE2 allow the selective anodic detection of CO at WE1 (+0.2 V vs Ag/AgCl) and that of NO at WE2 (+0.75 V vs Ag/AgCl) with sufficient sensitivity. Fluorinated xerogel coating on this dual electrode provides exclusive selectivity over common biological interferents, along with fast response time. The miniaturized size (end plane diameter < 300 μm) and tapered needle-like sensor geometry make the sensor become insertable into biological tissues. The sensor is applied to simultaneously monitor dynamic changes of NO and CO levels in a living rat brain under acute seizure condition induced by 4-aminopyridine in cortical tissue near the area of seizure induction. In-tissue measurement shows clearly defined patterns of NO/CO changes, directly correlated with observed LFP signal. Current study verifies the feasibility of a newly developed NO/CO dual sensor for real-time fast monitoring of intimately connected NO and CO dynamics. PMID:26855261

A differential pulse polarographic method was developed for acrolein. It is based on electrochemical reduction of acrolein at the dropping mercury electrode. With this method, acrolein can be quantitated in natural and condenser cooling waters at concentrations of 0.05 to 0.5 mg/...

In this paper, we report the fabrication of a dual microsensor for sensing nitric oxide (NO) and calcium ions (Ca(2+)) and its application for simultaneous NO/Ca(2+) measurements in living rat kidney tissue. NO and Ca(2+) have very important physiological functions and are both intricately involved in many biological processes. The dual NO/Ca(2+) sensor is prepared based on a dual recessed electrode possessing Pt (diameter, 25 μm) and Ag (diameter, 76 μm) microdisks. The Pt disk surface (WE1) is electrodeposited with porous Pt black and then coated with fluorinated xerogel; and used for amperometric sensing of NO. The Ag disk surface (WE2) is chloridated to AgCl, followed by silanization and then Ca(2+) selective membrane loading; and used for potentiometric sensing of Ca(2+). The dual sensor exhibits high sensitivity of WE1 to NO (40.8 ± 6.5 pA μM(-1), n = 10) and reliable Nerntian response of WE2 to Ca(2+) changes (25.7 ± 0.5 mV pCa(-1), n = 10) with excellent selectivity to only NO and Ca(2+) over common interferents and reliable stability (up to ∼4 h tissue experiment). The prepared sensor is employed for real-time monitoring of the dynamic changes of NO and Ca(2+) levels of a rat kidney, which is induced by the administration of 10 mM l-N(G)-nitroarginine methyl ester (l-NAME, a NO synthase inhibitor). Due to the small sensor dimension, location-dependent analyses of NO and Ca(2+) are carried out at two different regions of a kidney (renal medulla and cortex). Higher NO and Ca(2+) levels are observed at the medulla than at the cortex. This study verifies the feasibility for real-time monitoring of intimately connected Ca(2+) and endogenous NO production; and also for localized concentration assessments of both NO and Ca(2+). PMID:26606650

technologies were chosen. The MEMS-Sensors are acceleration-, tilt- and barometric pressure sensors. The positionsensors are draw wire and linear displacement transducers. In first laboratory tests the accuracy and resolution were investigated. The tests showed good results for all sensors. For example tilt-movements can be monitored with an accuracy of +/- 0,06° and a resolution of 0,1°. With the displacement transducer change in length of >0,1mm is possible. Apart from laboratory tests, field tests in South France and Germany were done to prove data stability and movement detection under real conditions. The results obtained were very satisfying, too. In the next step the combination of numerous sensors (sensor fusion) of the same type (redundancy) or different types (complementary) was researched. Different experiments showed that there is a high concordance between identical sensor-types. According to different sensor parameters (sensitivity, accuracy, resolution) some sensor-types can identify changes earlier. Taking this into consideration, good correlations between different kinds of sensors were achieved, too. Thus the experiments showed that combination of sensors is possible and this could improve the detection of movement and movement rate but also outliers. Based on this results various algorithms were setup that include different statistical methods (outlier tests, testing of hypotheses) and procedures from decision theories (Hurwicz-criteria). These calculation formulas will be implemented in the spatial data infrastructure (SDI) for the further data processing and validation. In comparison with today existing mainly punctually working monitoring systems, the application of wireless sensor networks in combination with low-cost, but precise micro-sensors provides an inexpensive and easy to set up monitoring system also in large areas. The correlation of same but also different sensor-types permits a good data control. Thus the sensor fusion is a promising tool

In this paper, we first report the construction of Nafion/glucose oxidase (GOD)/xylose dehydrogenase displayed bacteria (XDH-bacteria)/multiwalled carbon nanotubes (MWNTs) modified electrode for simultaneous voltammetric determination of D-glucose and D-xylose. The optimal conditions for the immobilized enzymes were established. Both enzymes retained their good stability and activities. In the mixture solution of D-glucose and D-xylose containing coenzyme NAD⁺ (the oxidized form of nicotinamide adenine dinucleotide), the Nafion/GOD/XDH-bacteria/MWNTs modified electrode exhibited quasi-reversible oxidation-reduction peak at -0.5 V (vs. saturated calomel electrode, SCE) originating from the catalytic oxidation of D-glucose, and oxidation peak at +0.55 V(vs. SCE) responding to the oxidation of NADH (the reduced form of nicotinamide adenine dinucleotide) by the carbon nanotubes, where NADH is the resultant product of coenzyme NAD⁺ involved in the catalysis of D-xylose by XDH-displayed bacteria. For the proposed biosensor, cathodic peak current at -0.5 V was linear with the concentration of D-glucose within the range of 0.25-6 mM with a low detection limit of 0.1 mM D-glucose (S/N=3), and the anodic peak current at +0.55 V was linear with the concentration of d-xylose in the range of 0.25∼4 mM with a low detection limit of 0.1 mM D-xylose (S/N=3). Further, D-xylose and D-glucose did not interfere with each other. 300-fold excess saccharides including D-maltose, D-galactose, D-mannose, D-sucrose, D-fructose, D-cellobiose, and 60-fold excess L-arabinose, and common interfering substances (100-fold excess ascorbic acid, dopamine, uric acid) as well as 300-fold excess D-xylitol did not affect the detection of D-glucose and D-xylose (both 1 mM). Therefore, the proposed biosensor is stable, specific, reproducible, simple, rapid and cost-effective, which holds great potential in real applications. PMID:23202346

Vitamin B9 or folic acid is an important food supplement with wide clinical applications. Due to its importance and its side effects in pregnant women, fast determination of this vitamin is very important. In this study we present a new fast and sensitive voltammetric sensor for the analysis of trace levels of vitamin B9 using a carbon paste electrode (CPE) modified with 1,3-dipropylimidazolium bromide (1,3-DIBr) as a binder and ZnO/CNTs nanocomposite as a mediator. The electro-oxidation signal of vitamin B9 at the surface of the 1,3-DIBr/ZnO/CNTs/CPE electrode appeared at 800 mV, which was about 95 mV less positive compared to the corresponding unmodified CPE. The oxidation current of vitamin B9 by square wave voltammetry (SWV) increased linearly with its concentration in the range of 0.08–650 μM. The detection limit for vitamin B9 was 0.05 μM. Finally, the utility of the new 1,3-DIBr/ZnO/CNTs/CPE electrode was tested in the determination of vitamin B9 in food and pharmaceutical samples. PMID:27231909

Vitamin B₉ or folic acid is an important food supplement with wide clinical applications. Due to its importance and its side effects in pregnant women, fast determination of this vitamin is very important. In this study we present a new fast and sensitive voltammetric sensor for the analysis of trace levels of vitamin B₉ using a carbon paste electrode (CPE) modified with 1,3-dipropylimidazolium bromide (1,3-DIBr) as a binder and ZnO/CNTs nanocomposite as a mediator. The electro-oxidation signal of vitamin B₉ at the surface of the 1,3-DIBr/ZnO/CNTs/CPE electrode appeared at 800 mV, which was about 95 mV less positive compared to the corresponding unmodified CPE. The oxidation current of vitamin B₉ by square wave voltammetry (SWV) increased linearly with its concentration in the range of 0.08-650 μM. The detection limit for vitamin B₉ was 0.05 μM. Finally, the utility of the new 1,3-DIBr/ZnO/CNTs/CPE electrode was tested in the determination of vitamin B₉ in food and pharmaceutical samples. PMID:27231909

A novel efficient differential pulse voltammetric (DPV) method for determination gallic acid (GA) was developed by using an electrochemical sensor based on [Cu2tpmc](ClO4)4 immobilized in PVC matrix and coated on graphite (CGE) or classy carbon rod (CGCE). The proposed method is based on the gallic acid oxidation process at formed [Cu2tpmcGA](3+) complex at the electrode surface. The complexation was explored by molecular modeling and DFT calculations. Voltammograms for both sensors, recorded in a HNO3 as a supporting electrolyte at pH 2 and measured in 2.5×10(-7) to 1.0×10(-4) M of GA, resulted with two linear calibration curves (for higher and lower GA concentration range). The detection limit at CGE was 1.48×10(-7) M, while at CGCE was 4.6×10(-6) M. CGE was successfully applied for the determination of the antioxidant capacity based on GA equivalents for white, rosé and red wine samples. PMID:25476338

Herein we describe the development, characterization and application of an electrochemical sensor based on the use of Nafion/MWCNT-modified screen-printed carbon electrodes (SPCEs) for the voltammetric detection of the anti-tuberculosis (anti-TB) drug ethambutol (ETB). The electrochemical behaviour of the drug at the surface of the developed Nafion/MWCNT-SPCEs was studied through cyclic voltammetry (CV) and square wave voltammetry (SWV) techniques. Electrochemical impedance spectroscopy (EIS) and scanning electron microscopy (SEM) were employed to characterize the modified surface of the electrodes. Results showed that, compared to both unmodified and MWCNTs-modified SPCEs, negatively charged Nafion/MWCNT-SPCEs remarkably enhanced the electrochemical sensitivity and selectivity for ETB due to the synergistic effect of the electrostatic interaction between cationic ETB molecules and negatively charged Nafion polymer and the inherent electrocatalytic properties of both MWCNTs and Nafion. Nafion/MWCNT-SPCEs provided excellent biocompatibility, good electrical conductivity, low electrochemical interferences and a high signal-to-noise ratio, providing excellent performance towards ETB quantification in microvolumes of human urine and human blood serum samples. The outcomes of this paper confirm that the Nafion/MWCNT-SPCE-based device could be a potential candidate for the development of a low-cost, yet reliable and efficient electrochemical portable sensor for the low-level detection of this antimycobacterial drug in biological samples. PMID:27376291

In this paper, a novel strategy was proposed to prepare ion-imprinted polymer (IIP) on the surface of reduced graphene oxide (RGO). Polymerization was performed using methacrylic acid (MAA) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, 2,2'-((9E,10E)-1,4-dihydroxyanthracene-9,10-diylidene) bis(hydrazine-1-carbothioamide) (DDBHCT) as the chelating agent and ammonium persulfate (APS) as initiator, via surface imprinted technique. The RGO-IIP was characterized by means of Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The electrochemical procedure was based on the accumulation of Hg(II) ions at the surface of a modified glassy carbon electrode (GCE) with RGO-IIP. The prepared RGO-IIP sensor has higher voltammetric response compared to the non-imprinted polymer (NIP), traditional IIP and RGO. The RGO-IIP modified electrode exhibited a linear relationship toward Hg(II) concentrations ranging from 0.07 to 80 μg L(-1). The limit of detection (LOD) was found to be 0.02 μg L(-1) (S/N=3), below the guideline value from the World Health Organization (WHO). The applicability of the proposed electrochemical sensor to determination of mercury(II) ions in different water samples was reported. PMID:27040231

Biochar is a carbonaceous material similar produced by pyrolysis of biomass under oxygen-limited conditions. Pyrolysis temperature is an important parameter that can alters biochar characteristics (e.g. surface area, pore size distribution and surface functional groups) and affects it efficacy for adsorption of several probes. In this work, biochar samples have been prepared from castor oil cake using different temperatures of pyrolysis (200-600°C). For the first time, a voltammetric procedure based on carbon paste modified electrode (CPME) was used to investigate the effect of temperature of pyrolysis on the adsorptive characteristics of biochar for Pb(II), Cd(II) and Cu(II) ions. Besides the electrochemical techniques, several characterizations have been performed to evaluate the physicochemical properties of biochar in function of the increase of the pyrolysis temperature. Results suggest that biochar pyrolized at 400°C (BC400) showed a better potential for ions adsorption. The CPME modified with BC400 showed better relative current signal with adsorption affinity: Pb(II)>Cd(II)>Cu(II). Kinetic studies revealed that the pseudo-second order model describes more accurately the adsorption process suggesting that the surface reactions control the adsorption rate. Values found for amount adsorbed were 15.94±0.09; 4.29±0.13 and 2.38±0.39μgg(-1) for Pb(II), Cd(II) and Cu(II) ions, respectively. PMID:27469040

In this paper, we carried out detailed electrochemical studies of epitaxial graphene (EG) using inner-sphere and outer-sphere redox mediators. The EG sample was anodized systematically to investigate the effect of edge plane defects on the heterogeneous charge transfer kinetics and capacitive noise. We found that anodized EG, consisting of oxygen-related defects, is a superior biosensing platform for the detection of nucleic acids, uric acids (UA), dopamine (DA), and ascorbic acids (AA). Mixtures of nucleic acids (A, T, C, G) or biomolecules (AA, UA, DA) can be resolved as individual peaks using differential pulse voltammetry. In fact, an anodized EG voltammetric sensor can realize the simultaneous detection of all four DNA bases in double stranded DNA (dsDNA) without a prehydrolysis step, and it can also differentiate single stranded DNA from dsDNA. Our results show that graphene with high edge plane defects, as opposed to pristine graphene, is the choice platform in high resolution electrochemical sensing. PMID:20712323

A novel voltammetric sensor based on glassy carbon electrode (GCE) modified with a thin film of multi-walled carbon nanotubes (MWCNTs) coated with an electropolymerized layer of tiron-doped polypyrrole was developed and the resulting electrode was applied for the determination of acyclovir (ACV). The surface morphology and property of the modified electrode were characterized by field emission scanning electron microscopy and electrochemical impedance spectroscopy techniques. The electrochemical performance of the modified electrode was investigated by means of linear sweep voltammetry (LSV). The effect of several experimental variables, such as pH of the supporting electrolyte, drop size of the cast MWCNTssuspension, number of electropolymerization cycles and accumulation time was optimized by monitoring the LSV response of the modified electrode toward ACV. The best response was observed at pH7.0 after accumulation at open circuit for 160 s. Under the optimized conditions, a significant electrochemical improvement was observed toward the electrooxidation of ACV on the modified electrode surface relative to the bare GCE, resulting in a wide linear dynamic range (0.03-10.0μ M) and a low detection limit (10.0 nM) for ACV. Besides high sensitivity, the sensor represented high stability and good reproducibility for ACV analysis, and provided satisfactory results for the determination of this compound in pharmaceutical and clinical preparations. PMID:26042700

The paper describes the fabrication and application of a novel sensor (a boron-doped diamond electrode modified with Nafion and lead films) for the simultaneous determination of paracetamol and ascorbic acid by differential pulse voltammetry. The main advantage of the lead film and polymer covered boron-doped diamond electrode is that the sensitivity of the stripping responses is increased and the separation of paracetamol and ascorbic acid signals is improved due to the modification of the boron-doped diamond surface by the lead layer. Additionally, the repeatability of paracetamol and ascorbic acid signals is improved by the application of the Nafion film coating. In the presence of oxygen, linear calibration curves were obtained in a wide concentration range from 5×10(-7) to 2×10(-4) mol L(-1) for paracetamol and from 1×10(-6) to 5×10(-4) mol L(-1) for ascorbic acid. The analytical utility of the differential pulse voltammetric method elaborated was tested in the assay of paracetamol and ascorbic acid in commercially available pharmaceutical formulations and the method was validated by high performance liquid chromatography coupled with diode array detector. PMID:25127609

Herein we describe the development, characterization and application of an electrochemical sensor based on the use of Nafion/MWCNT-modified screen-printed carbon electrodes (SPCEs) for the voltammetric detection of the anti-tuberculosis (anti-TB) drug ethambutol (ETB). The electrochemical behaviour of the drug at the surface of the developed Nafion/MWCNT-SPCEs was studied through cyclic voltammetry (CV) and square wave voltammetry (SWV) techniques. Electrochemical impedance spectroscopy (EIS) and scanning electron microscopy (SEM) were employed to characterize the modified surface of the electrodes. Results showed that, compared to both unmodified and MWCNTs-modified SPCEs, negatively charged Nafion/MWCNT-SPCEs remarkably enhanced the electrochemical sensitivity and selectivity for ETB due to the synergistic effect of the electrostatic interaction between cationic ETB molecules and negatively charged Nafion polymer and the inherent electrocatalytic properties of both MWCNTs and Nafion. Nafion/MWCNT-SPCEs provided excellent biocompatibility, good electrical conductivity, low electrochemical interferences and a high signal-to-noise ratio, providing excellent performance towards ETB quantification in microvolumes of human urine and human blood serum samples. The outcomes of this paper confirm that the Nafion/MWCNT-SPCE-based device could be a potential candidate for the development of a low-cost, yet reliable and efficient electrochemical portable sensor for the low-level detection of this antimycobacterial drug in biological samples. PMID:27376291

An analytical procedure fit for the simultaneous determination of copper (II), chromium(VI), thallium(I), lead(II), tin(II), antimony(III), and zinc(II) by square wave anodic stripping voltammetry (SWASV) in three interdependent environmental matrices involved in foods and food chain as meals, cereal plants and soils is described. The digestion of each matrix was carried out using a concentrated HCl-HNO3-H2SO4 (meals and cereal plants) and HCl-HNO3 (soils) acidic attack mixtures. 0.1 mol/L dibasic ammonium citrate pH 8.5 was employed as the supporting electrolyte. The voltammetric measurements were carried out using, as working electrode, a stationary hanging mercury drop electrode (HMDE) and a platinum electrode and an Ag/AgCl/KClsat electrode as auxiliary and reference electrodes, respectively. The analytical procedure was verified by the analyses of the standard reference materials: Wholemeal BCR-CRM 189, Tomato Leaves NIST-SRM 1573a and Montana Soil Moderately Elevated Traces NIST-SRM 2711. For all the elements in the certified matrix, the precision as repeatability, expressed as relative standard deviation (Sr %) was lower than 5%. The accuracy, expressed as percentage relative error (e %) was of the order of 3-7%, while the detection limits were in the range 0.015-0.103 microg/g. Once set up on the standard reference materials, the analytical procedure was transferred and applied to commercial meal samples, cereal plants and soils samples drawn in sites devoted to agricultural practice. A critical comparison with spectroscopic measurements is also discussed. PMID:17822223

An easy, rapid and selective adsorptive stripping voltammetry (AdSV) method for the determination of vincamine in its formulation and human serum was developed and validated. It was based on the oxidation of the drug onto a Nujol-based carbon paste electrode. The stripping step was carried out by using a square-wave (SW) potential-time voltammetric excitation signal. The optimal experimental variables as well as accumulation parameters were investigated as; frequency f=120 Hz, scan increment DeltaE(i)=10 mV, pulse-amplitude DeltaE(a)=25 mV and an accumulation potential E(acc) of 0.0 V using a Britton-Robinson (B-R) universal buffer of pH 5 as a supporting electrolyte. After validation of the described method, it was applied for determination of vincamine in its formulation and human serum. Mean recovery of 100.41+/-0.74 (n=5) was achieved for assay of vincamine in Oxybral capsules. Limits of detection and quantitation of 6.0 x 10(-9) M (2.20 ng ml(-1)) and 2 x 10(-8) M (7.33 ng ml(-1)) vincamine were achieved in human serum with a mean recovery of 99.5+/-1.79%, without prior extraction of the drug. No interferences were observed in formulation and/or human serum. Due to high sensitivity and specificity of the developed method, it was successfully applied for evaluating some pharmacokinetic parameters of two healthy volunteers after administration of a single oral Oxybral capsule. PMID:19043234

The use of anthraquinone and its derivatives, notably the sulfonate and disulfonate salts, for the detection of DNA via electrochemical techniques, has been the focus of a number of recent articles. This study provides a quantitative model of the two redox systems of anthraquinone-2,6-disulfonate and anthraquinone-2-sulfonate, over the full aqueous pH range (0-13); the model is based upon the theoretical "scheme of squares" for a 2H(+), 2e(-) system, as first proposed by Jacq (Jacq, J. J. Electroanal. Chem. 1971, 29, 149-180). The effect of pH and ionic strength on the observed cyclic voltammetry was investigated experimentally. The variation of the electrochemical response with proton concentration was modeled through use of the commercially available simulation software, DIGISIM; the system was successfully fitted with attention to voltammetric peak height, position, width, and shape. The model demonstrates how the pK(a) values of the anthraquinone intermediates dominate the observed pH dependence of the voltammetry. At high pH (above pH 12), a simple EE process is found to occur. As the pH decreases, the formation of other protonated species becomes possible; this not only causes a Nernstian shift in the measured electrochemical potential for the redox couple but also results in changes in the mechanistic pathway. At pH 10, an EECC process dominates, as the pH is further lowered into the range 4-7, the overall mechanism is an ECEC process, and finally a CECE mechanism operates at around pH 1 and below. This work provides physical insight into the complex mechanistic pathways involved and will aid the future development of more sophisticated and accurate anthraquinone based DNA sensors. PMID:20196578

Atomic absorption spectrometry and inductively coupled plasma-mass spectrometry are widely used for determination of heavy metals due to their low detection limits. However, they are not applicable to on-site measurements of heavy metals as bulky equipment, and highly skilled laboratory staffs are needed as well. In this study, a novel analytical method using a rotary disc voltammetric (RDV) sensor has been successfully designed, fabricated and characterized for semi-continuous and on-site measurements of trace levels of Pb(II) in non-deoxygenating solutions. The square wave anodic stripping voltammetry was used to improve the sensitivity of the Pb(II) detection level with less than 10nM (2μgL(-1)). The RDV sensor has 24-sensing holes to measure concentrations of Pb(II) semi-continuously at sampling sites. Each sensing hole consists of a silver working electrode, an integrated silver counter, and a quasi-reference electrode, which requires only a small amount of samples (<30μL) for measurement of Pb(II) without disturbing and/or clogging the sensing environment. In addition, the RDV sensor showed a correlation coefficient of 0.998 for the Pb(II) concentration range of 10nM-10μM at the deposition time of 180s and its low detection limit was 6.19nM (1.3μgL(-1)). These results indicated that the advanced monitoring technique using a RDV sensor might provide environmental engineers with a reliable way for semi-continuous and on-site measurements of Pb(II). PMID:26058555

Theoretical and experimental approaches to characterizing nanoelectrode (NE) ensembles of ultramicroelectrode dimensions (UME-NEEs) as a function of fraction of active area and random NE distribution are described. UME-NEEs were fabricated by addressing microregions of a gold-filled polycarbonate membrane through the UMEs of an underlying microfabricated addressable array. Results of Comsol Multiphysics 3D simulations based on randomly spaced NEs of 15 nm radius on a UME disk geometry of radii up to 5 μm are shown for steady-state voltammetry (SSV) and scanning electrochemical microscopy (SECM) experiments. Analytical equations were developed to describe the diffusion-limited steady-state current and steady-state voltammogram at an UME-NEE. These equations are shown to be in good agreement with the simulations and enabled evaluation of experimental SSVs. Comparison of experimental and simulated SECM approach curves, images, and tip voltammograms enabled the fraction of active area and distribution of NEs to be visualized and determined for individual UME-NEEs. Gold UME-NEEs are shown to be unique platforms for electrodeposition in forming nanoparticle electrodes (UME-NPEs). Electrocatalysis results for the oxygen reduction reaction (ORR) on Pt UME-NPEs in 0.1 M H2SO4 are also shown. PMID:25495486

An electrochemical sensor was prepared by the modification of a glassy carbon electrode (GCE) with carbon nanotubes (CNTs) and nanoparticles of antimony tin oxide (ATO). The surface layer was characterized by scanning electronmicroscopy (SEM), energy dispersive X-ray diffraction method (EDX) and ATR FT-IR spectroscopy. The proposed electrode was assessed in respect to the electro-oxidation of ractopamine. Compared with a bare GCE and a GCE electrode modified with CNTs, the ATONPs/CNTs/GCE exhibited a great catalytic activity towards the oxidation of ractopamine with a well-defined anodic peak at 600 mV. The current response was linear with the concentration of ractopamine over the range from 10 to 240 nM with a detection limit of 3.3 nM. The proposed electrode enabled the selective determination of ractopamine in the presence of high concentrations of ascorbic acid (AA), dopamine (DA) and uric acid (UA). The proposed electrode was successfully applied for the determination of ractopamine in feed and urine samples. The sensitive and selective determination of ractopamine makes the developed method of great interest for monitoring its therapeutic use and doping control purposes. PMID:26652385

In the present work, graphene sheets (GS) and multiwall carbon nanotubes (MWCNTs) were dispersed in the mixed solution of cyclodextrin (CD) and cyclodextrin prepolymer (pre-CD) and were used as modifier to fabricate chemical modified electrode to simultaneous detect dopamine (DA), ascorbic acid (AA) and nitrite (NO2(-)). CD cross-linked pre-CD (CDP) displays excellent film forming ability, which made the electrode stable. Comparing with CDP-GS, CDP-MWCNTs and CDP-GS-MWCNTs modified electrodes, the CDP-GS-MWCNTs displays higher catalytic activity and selectivity toward the oxidation of DA, AA and NO2(-), revealing that MWCNTs effectively inhibited the stacking of individual GS and enhanced the utilization of GS based composites. The host-guest chemical reaction ability of CD and π-π stacking interaction between detected molecules and GS-MWCNTs surface were considered as the main reasons of the successfully simultaneous detection of DA, AA and NO2(-). Cyclic voltammetry (CV), scanning electron microscopy (SEM) and different pulse voltammetry (DPV) were employed to characterize the biosensor. The linear response range for AA, DA and NO2(-) were 5 μM-0.48 mM, 0.15-21.65 μM and 5 μM-6.75 mM, respectively and the detection limits were 1.65 μM, 0.05 μM and 1.65 μM. PMID:21497078

Electrochemical behavior of artificial antioxidant, butylated hydroxyanisole (BHA), was investigated at a glassy carbon electrode modified with poly L- cysteine [poly (L- Cys/GCE)]. BHA exhibits a pair of well - defined redox peak on L- cysteine modified GCE with Epa = 69 mV and Epc = 4 mV. The modified electrode showed good electrocatalytic activity towards the oxidation of BHA under optimal conditions and exhibited a linear response in the range from 1.0 × 10(-5) to 1.0 × 10(-6) M with a correlation coefficient of 0.998. The limit of detection was found to be 4.1 × 10(-7) M. The kinetics parameters of the proposed sensor such as heterogeneous electron transfer rate, k s , and charge transfer coefficient,α, was calculated and found to be 1.20 s(-1) and 0.575 respectively. The average surface concentration of BHA on the surface of poly (L- Cys/GCE) was calculated to be 3.18 × 10(-4) mol cm(-2). The analytical utility of the proposed sensor was evaluated by the successful determination of BHA in coconut oil and sesame oil samples. PMID:26396421

The effects of various procedures which modify consciousness were studied on the extracellular concentration of ascorbic acid (AA), 3,4-dihydroxyphenylacetic acid (DOPAC) and 5-hydroxyindolacetic acid (5HIAA) in rat striatum, as measured by differential pulse voltammetry (DPV) with electrically pretreated carbon fibre micro-electrodes (CFE). Recovery from anaesthesia (produced by 500 mg/kg i.p. chloral hydrate) was accompanied by a six-fold increase in extracellular striatal AA levels, while negligible changes in DOPAC and 5HIAA occurred. Following complete recovery from anaesthesia, the animals were re-injected with the same dose of anaesthetic which specifically reduced AA levels by 90% (DOPAC levels were unchanged and 5HIAA concentrations slightly reduced). In conscious rats, the neuroleptic haloperidol (1 mg/kg i.p., n = 5) and the minor tranquillizer diazepam (10 mg/kg i.p., n = 5), both considered as behaviourally depressant drugs, reduced extracellular AA levels to 50% of controls. The psychomotor stimulant D-amphetamine (1 mg/kg i.p., n = 5) increased AA levels by 90% over controls. Stress activation of animals (handling for 10 min, n = 10) also produced a transient, significant increase (180% of control values) in this striatal parameter. Taken together with previous reports, our results suggest a close relationship between the state of consciousness and extracellular AA levels in the rat striatum and that this relationship appears to be more correlated to AA as no such clear interdependence was noted between the levels of consciousness and extracellular striatal DOPAC or 5HIAA. PMID:1381092

A combination of different methods was applied to investigate the occurrence of anaerobic processes in aerated activated sludge. Microsensor measurements (O{sub 2}, NO{sub 2}{sup {minus}}, NO{sub 3}{sup {minus}}, and H{sub 2}S) were performed on single sludge flocs to detect anoxic niches, nitrate reduction, or sulfate reduction on a microscale. Incubations of activated sludge with {sup 15}NO{sub 3}{sup {minus}} and {sup 35}SO{sub 4}{sup 2{minus}} were used to determine denitrification and sulfate reduction rates on a batch scale. In four of six investigated sludges, no anoxic zones developed during aeration, and consequently denitrification rates were very low. However, in two sludges anoxia in flocs coincided with significant denitrification rates. Sulfate reduction could not be detected in any sludge in either the microsensor or the batch investigation, not even under short-term anoxic conditions. In contrast, the presence of sulfate-reducing bacteria was shown by fluorescence in situ hybridization with 16S rRNA-targeted oligonucleotide probes and by PCR-based detection of genes coding for the dissimilatory sulfite reductase. A possible explanation for the absence of advection, i.e., facilitated by flow through pores and channels. This possibility is suggested by the irregularity of some oxygen profiles and by confocal laser scanning microscopy of the three-dimensional floc structures, which showed that flocs from the two sludges in which anoxic zones were found were apparently denser than flocs from the other sludges.

An apparatus and method is described for electrochemical analysis of elements in solution. An auxiliary electrode, a reference electrode, and five working electrodes are positioned in a container containing a sample solution. The working electrodes are spaced apart evenly from each other and the auxiliary electrode to minimize any inter-electrode interference that may occur during analysis. An electric potential is applied between the auxiliary electrode and each of the working electrodes. Simultaneous measurements taken of the current flow through each of the working electrodes for each given potential in a potential range are used for identifying chemical elements present in the sample solution and their respective concentrations. Multiple working electrodes enable a more positive identification to be made by providing unique data characteristic of chemical elements present in the sample solution.

Presents three activities: (1) investigating succession in a schoolground; (2) investigating oak galls; and (3) making sun prints (photographs made without camera or darkroom). Each activity includes a list of materials needed and procedures used. (JN)

A series of four activities are presented to enhance students' abilities to appreciate and use trigonometry as a tool in problem solving. Activities cover problems applying the law of sines, the law of cosines, and matching equivalent trigonometric expressions. A teacher's guide, worksheets, and answers are provided. (MDH)

In view of alkaline water electrolysis, the activities for the hydrogen evolution reaction of nanocrystalline Fe-based electrode materials were investigated and compared with the activities of polycrystalline Fe and Ni. Electrochemical methods were used to elucidate the overpotential value, the charge transfer resistance and the double layer capacity. Structural properties of the electrode surface were determined with SEM, XRD and XPS analyses. Thus, a correlation between electrochemical and structural parameters was found. In this context, we report on a cyclic voltammetricactivation procedure which causes a significant increase of the surface area of Fe-based electrodes leading to a boost in effective activity of the activated electrodes. It was found that the intrinsic activity of activated Fe-based electrodes is very high due to the formation of a nanocrystalline surface layer. In contrast, the activation procedure influences only the intrinsic activity of the Ni electrodes without the formation of a porous surface layer.

Presents an activity in which students collect and organize data from a real-world simulation of the scientific concept of half life. Students collect data using a marble sifter, analyze the data using a graphing calculator, and determine an appropriate mathematical model. Includes reproducible worksheets. (MDH)

A fast and non-destructive voltammetric method to detect cocaine in confiscated samples based on carbon paste electrode modified with methoxy-substituted N,N'-ethylene-bis(salcylideneiminato)uranyl(VI)complexes, [UO2(X-MeOSalen)(H2O)].H2O, where X corresponds to the positions 3, 4 or 5 of the methoxy group on the aromatic ring, is described. The electrochemical behavior of the modified electrode and the electrochemical detection of cocaine were investigated using cyclic voltammetry. Using 0.1 mol·L−1 KCl as supporting-electrolyte, a concentration-dependent, well-defined peak current for cocaine at 0.62 V, with an amperometric sensitivity of 6.25 × 104 μA·mol·L−1 for cocaine concentrations ranging between 1.0 × 10−7 and 1.3 × 10−6 mol·L−1 was obtained. Chemical interference studies using lidocaine and procaine were performed. The position of the methoxy group affects the results, with the 3-methoxy derivative being the most sensitive. PMID:23771156

A new thin-film heat flux gage has been fabricated specifically for severe high temperature operation using platinum and platinum-10 percent rhodium for the thermocouple elements. Radiation calibrations of this gage were performed at the AEDC facility over the available heat flux range (approx. 1.0 - 1,000 W/cu cm). The gage output was linear with heat flux with a slight increase in sensitivity with increasing surface temperature. Survivability of gages was demonstrated in quench tests from 500 C into liquid nitrogen. Successful operation of gages to surface temperatures of 750 C has been achieved. No additional cooling of the gages is required because the gages are always at the same temperature as the substrate material. A video of oxyacetylene flame tests with real-time heat flux and temperature output is available.

The fabrication of novel multielement microelectrode array sensors is reported. With regard to individual array elements, two main concepts are pursued. One involves the use of relatively non-selective microelectrode elements, coupled with pattern recognition methods, for data analysis. This strategy is most applicable when prior knowledge about the chemical environment is limited, or when mainly qualitative information is sought. The second concept involves the development of arrays containing intrinsically more selective microelectrode elements. Our main concern here is the determination of specific contaminants. Most of our current emphasis is in the selection and development of appropriate elements for microelectrode arrays of this type, with a goal of quantitative analysis for a variety of compounds and elements. Other efforts are concerned with defining the behavior of microelectrodes and devising mass fabrication methods for these sensors. Two designs for the arrays are discussed, one employing photolithographic fabrication methods and another in which individual microelectrodes are encased in glass. Potential applications for these sensors include monitoring for toxic contaminants in natural waters, monitoring waste streams, and process control.

Periodic silicon nanostructures can be used for different kinds of gas sensors depending on the analyte concentration. First we present an optical gas sensor based on the classical non-dispersive infrared technique for ppm-concentration using ultra-compact photonic crystal gas cells. It is conceptually based on low group velocities inside a photonic crystal gas cell and anti-reflection layers coupling light into the device. Experimentally, an enhancement of the CO2 infrared absorption by a factor of 2.6 to 3.5 as compared to an empty cell, due to slow light inside a 2D silicon photonic crystal gas cell, was observed; this is in excellent agreement with numerical simulations. In addition we report on silicon nanotip arrays, suitable for gas ionization in ion mobility microspectrometers (micro-IMS) having detection ranges in principle down to the ppt-range. Such instruments allow the detection of explosives, chemical warfare agents, and illicit drugs, e.g., at airports. We describe the fabrication process of large-scale-ordered nanotips with different tip shapes. Both silicon microstructures have been fabricated by photoelectrochemical etching of silicon.

This work is motivated by a demand for inexpensive, robust and reliable biochemical sensors with high signal reproducibility and long-term-stable sensitivity, especially for medical applications. Micro-fabricated sensors can provide continuous monitoring and on-line control of analyte concentrations in ambient aqueous solutions. The piezoresistive biochemical sensor containing a special biocompatible polymer (hydrogel) with a sharp volume phase transition in the neutral physiological pH range near 7.4 can detect a specific analyte, for example glucose. Thereby the hydrogel-based biochemical sensors are useful for the diagnosis and monitoring of diabetes. The response of the glucosesensitive hydrogel was studied at different regimes of the glucose concentration change and of the solution supply. Sensor response time and accuracy with which a sensor can track gradual changes in glucose was estimated. Additionally, the influence of various recommended sterilization methods on the gel swelling properties and on the mechano-electrical transducer of the pH-sensors has been evaluated in order to choose the most optimal sterilization method for the implantable sensors. It has been shown that there is no negative effect of gamma irradiation with a dose of 25.7 kGy on the hydrogel sensitivity. In order to achieve an optimum between sensor signal amplitude and sensor response time, corresponding calibration and measurement procedures have been proposed and evaluated for the chemical sensors.

Recognition of body posture and motion is an important physiological function that can keep the body in balance. Man-made motion sensors have also been widely applied for a broad array of biomedical applications including diagnosis of balance disorders and evaluation of energy expenditure. This paper reviews the state-of-the-art sensing components utilized for body motion measurement. The anatomy and working principles of a natural body motion sensor, the human vestibular system, are first described. Various man-made inertial sensors are then elaborated based on their distinctive sensing mechanisms. In particular, both the conventional solid-state motion sensors and the emerging non solid-state motion sensors are depicted. With their lower cost and increased intelligence, man-made motion sensors are expected to play an increasingly important role in biomedical systems for basic research as well as clinical diagnostics. PMID:22346595

Recognition of body posture and motion is an important physiological function that can keep the body in balance. Man-made motion sensors have also been widely applied for a broad array of biomedical applications including diagnosis of balance disorders and evaluation of energy expenditure. This paper reviews the state-of-the-art sensing components utilized for body motion measurement. The anatomy and working principles of a natural body motion sensor, the human vestibular system, are first described. Various man-made inertial sensors are then elaborated based on their distinctive sensing mechanisms. In particular, both the conventional solid-state motion sensors and the emerging non solid-state motion sensors are depicted. With their lower cost and increased intelligence, man-made motion sensors are expected to play an increasingly important role in biomedical systems for basic research as well as clinical diagnostics. PMID:22346595

Optofluidics is a relatively young research field able to create a tight synergy between optics and micro/nano-fluidics. The high level of integration between fluidic and optical elements achievable by means of optofluidic approaches makes it possible to realize an innovative class of sensors, which have been demonstrated to have an improved sensitivity, adaptability and compactness. Many developments in this field have been made in the last years thanks to the availability of a new class of low cost materials and new technologies. This review describes the Italian state of art on optofluidic devices for sensing applications and offers a perspective for further future advances. We introduce the optofluidic concept and describe the advantages of merging photonic and fluidic elements, focusing on sensor developments for both environmental and biomedical monitoring. PMID:25558989

The fabrication of novel multielement microelectrode array sensors is reported. With regard to individual array elements, two main concepts are pursued. One involves the use of relatively non-selective microelectrode elements, coupled with pattern recognition methods, for data analysis. This strategy is most applicable when prior knowledge about the chemical environment is limited, or when mainly qualitative information is sought. The second concept involves the development of arrays containing intrinsically more selective microelectrode elements. Our main concern here is the determination of specific contaminants. Most of our current emphasis is in the selection and development of appropriate elements for microelectrode arrays of this type, with a goal of quantitative analysis for a variety of compounds and elements. Other efforts are concerned with defining the behavior of microelectrodes and devising mass fabrication methods for these sensors. Two designs for the arrays are discussed, one employing photolithographic fabrication methods and another in which individual microelectrodes are encased in glass. Potential applications for these sensors include monitoring for toxic contaminants in natural waters, monitoring waste streams, and process control. 35 refs., 16 figs., 3 tabs.

The bottleneck in the development of chemical sensors is the design of the coatings for chemical recognition of the analyte. One pronounced method is to tailor supramolecular cavities for different analytes. Polyfunctional linkers or the embedding of these materials in a polymeric matrix can improve stability and response time of the sensor. An even more favorable method to synthesize chemically sensitive layers is realized by molecular imprinting, since a rigid polymer can be generated directly on the transducer of interest and may be included in its production process. The analyte of interest acts as a template during the polymerization process and is evaporated or extracted by suitable solvents. Due to the cavities formed this polymer enriches analyte molecules, which can be detected by mass- sensitive devices such as QMB or SAW resonators or by optical measurements. This procedure allows both the detection of polycyclic aromatic hydrocarbons (PAHs) with fluorescence or mass sensitive devices. If the print PAHs are varied the polymers are tuned to the desired analyte. The enrichment of solvent vapors or other uncolored specimen by the layer can also be followed by the embedding of carbenium ions used as optical labels.

The microbial community structure and spatial distribution of microorganisms and their in situ activities in anaerobic granules were investigated by 16S rRNA gene-based molecular techniques and microsensors for CH4, H2, pH, and the oxidation-reduction potential (ORP). The 16S rRNA gene-cloning analysis revealed that the clones related to the phyla Alphaproteobacteria (detection frequency, 51%), Firmicutes (20%), Chloroflexi (9%), and Betaproteobacteria (8%) dominated the bacterial clone library, and the predominant clones in the archaeal clone library were affiliated with Methanosaeta (73%). In situ hybridization with oligonucleotide probes at the phylum level revealed that these microorganisms were numerically abundant in the granule. A layered structure of microorganisms was found in the granule, where Chloroflexi and Betaproteobacteria were present in the outer shell of the granule, Firmicutes were found in the middle layer, and aceticlastic Archaea were restricted to the inner layer. Microsensor measurements for CH4, H2, pH, and ORP revealed that acid and H2 production occurred in the upper part of the granule, below which H2 consumption and CH4 production were detected. Direct comparison of the in situ activity distribution with the spatial distribution of the microorganisms implied that Chloroflexi contributed to the degradation of complex organic compounds in the outermost layer, H2 was produced mainly by Firmicutes in the middle layer, and Methanosaeta produced CH4 in the inner layer. We determined the effective diffusion coefficient for H2 in the anaerobic granules to be 2.66 × 10−5 cm2 s−1, which was 57% in water. PMID:17905889

Electrocatalytic activity of carbon (Vulcan XC-72) supported selenium-modified ruthenium, RuSex/C, nanoparticles for reduction of oxygen was enhanced through intentional decoration with iridium nanostructures (dimensions, 2-3 nm). The catalytic materials were characterized in oxygenated 0.5 mol dm-3 H2SO4 using cyclic and rotating ring disk voltammetric techniques as well as using transmission electron microscopy and scanning electron microscopy equipped with X-ray dispersive analyzer. Experiments utilizing gas diffusion electrode aimed at mimicking conditions existing in the low-temperature fuel cell. Upon application of our composite catalytic system, the reduction of oxygen proceeded at more positive potentials, and higher current densities were observed when compared to the behavior of the simple iridium-free system (RuSex/C) investigated under the analogous conditions. The enhancement effect was more pronounced than that one would expect from simple superposition of voltammetric responses for the oxygen reduction at RuSex/C and iridium nanostructures studied separately. Nanostructured iridium acted here as an example of a powerful catalyst for the reduction of H2O2 (rather than O2) and, when combined with such a moderate catalyst as ruthenium-selenium (for O2 reduction), it produced an integrated system of increased electrocatalytic activity in the oxygen reduction process. The proposed system retained its activity in the presence of methanol that could appear in a cathode compartment of alcohol fuel cell.

We report the redox properties of four star systems incorporating the 4-benzoyl-N-alkylpyridinium cation; the redox potential varies along the branches, but remains constant at fixed radii. Voltammetric analysis (cyclic voltammetry and differential pulse voltammetry) shows that only two of the three redox-active centers in the perimeter are electrochemically accessible during potential sweeps as slow as 20 mV/s and as fast as 10 V/s. On the contrary, both redox centers of a branch are accessible electrochemically within the same time frame. These results are discussed in terms of slow through-space charge transfer and the globular 3-D folding of the molecules.

Carnosine, homocarnosine, and anserine are present in high concentrations in the muscle and brain of many animals and humans. However, their exact function is not clear. The antioxidant activity of these compounds has been examined by testing their peroxyl radical-trapping ability at physiological concentrations. Carnosine, homocarnosine, anserine, and other histidine derivatives all showed antioxidant activity. All of these compounds showing peroxyl radical-trapping activity were also electrochemically active as reducing agents in cyclic voltammetric measurements. Furthermore, carnosine inhibited the oxidative hydroxylation of deoxyguanosine induced by ascorbic acid and copper ions. Other roles of carnosine, such as chelation of metal ions, quenching of singlet oxygen, and binding of hydroperoxides, are also discussed. The data suggest a role for these histidine-related compounds as endogenous antioxidants in brain and muscle. PMID:3362866

The complexation of new mixed thia-aza-oxa macrocycle viz., 2,12-dithio-5,9,14,18-tetraoxo-7,16-dithia-1,3,4,10,11,13-hexaazacyclooctadecane containing thiosemicarba-zone unit with a series of transition metals Co(II), Ni(II) and Cu(II) has been investigated, by different spectroscopic techniques. The structural features of the ligand have been studied by EI-mass, 1H NMR and IR spectral techniques. Elemental analyses, magnetic moment susceptibility, molar conductance, IR, electronic, and EPR spectral studies characterized the complexes. Electronic absorption and IR spectra of the complexes indicate octahedral geometry for chloro, nitrato, thiocyanato or acetato complexes. The dimeric and neutral nature of the sulphato complexes are confirmed from magnetic susceptibility and low conductance values. Electronic spectra suggests square-planar geometry for all sulphato complexes. The redox behaviour was studied by cyclic voltammetry, show metal-centered reduction processes for all complexes. The complexes of copper show both oxidation and reduction process. The redox potentials depend on the conformation of central atom in the macrocyclic complexes. Newly synthesized macrocyclic ligand and its transition metal complexes show markedly growth inhibitory activity against pathogenic bacterias and plant pathogenic fungi under study. Most of the complexes have higher activity than that of the metal free ligand.

In this study, 2-hydroxy-5-methoxyacetophenone thiosemicarbazone (HMAT) and its novel N(4) substituted derivatives were synthesized and characterized by different techniques. The optical band gap of the compounds and the energy of HOMO were experimentally examined by UV-vis spectra and cyclic voltammetry measurements, respectively. Furthermore, the conformational spaces of the compounds were scanned with molecular mechanics method. The geometry optimization, HOMO and LUMO energies, the energy gap of the HOMO-LUMO, dipole moment of the compounds were theoretically calculated by the density functional theory B3LYP/6-311++G(d,p) level. The minimal electronic excitation energy and maximum wavelength calculations of the compounds were also performed by TD-DFT//B3LYP/6-311++G(d,p) level of theory. Theoretically calculated values were compared with the related experimental values. The combined results exhibit that all compounds have good electron-donor properties which affect anti-proliferative activity. The cytotoxic effects of the compounds were also evaluated against HeLa (cervical carcinoma), MCF-7 (breast carcinoma) and PC-3 (prostatic carcinoma) cell lines using the standard MTT assay. All tested compounds showed antiproliferative effect having IC50 values in different range. In comparison with that of HMAT, it was obtained that while ethyl group on 4(N)-substituted position decreased in potent anti-proliferative effect, the phenyl group on the position increased in anti-proliferative effect for the tested cancer cell line. Considering the molecular energy parameters, the cytotoxicity activities of the compounds were discussed. PMID:25448971

In this study, 2-hydroxy-5-methoxyacetophenone thiosemicarbazone (HMAT) and its novel N(4) substituted derivatives were synthesized and characterized by different techniques. The optical band gap of the compounds and the energy of HOMO were experimentally examined by UV-vis spectra and cyclic voltammetry measurements, respectively. Furthermore, the conformational spaces of the compounds were scanned with molecular mechanics method. The geometry optimization, HOMO and LUMO energies, the energy gap of the HOMO-LUMO, dipole moment of the compounds were theoretically calculated by the density functional theory B3LYP/6-311++G(d,p) level. The minimal electronic excitation energy and maximum wavelength calculations of the compounds were also performed by TD-DFT//B3LYP/6-311++G(d,p) level of theory. Theoretically calculated values were compared with the related experimental values. The combined results exhibit that all compounds have good electron-donor properties which affect anti-proliferative activity. The cytotoxic effects of the compounds were also evaluated against HeLa (cervical carcinoma), MCF-7 (breast carcinoma) and PC-3 (prostatic carcinoma) cell lines using the standard MTT assay. All tested compounds showed antiproliferative effect having IC50 values in different range. In comparison with that of HMAT, it was obtained that while ethyl group on 4(N)-substituted position decreased in potent anti-proliferative effect, the phenyl group on the position increased in anti-proliferative effect for the tested cancer cell line. Considering the molecular energy parameters, the cytotoxicity activities of the compounds were discussed.

A commercially available sputtered bismuth screen-printed electrode (BispSPE) has been pioneeringly applied for the simultaneous determination of Cd(II) and Pb(II) ions in a certified groundwater sample by means of differential pulse anodic stripping voltammetry (DPASV) as an alternative to more conventional bismuth screen-printed carbon electrodes (BiSPCEs). BispSPEs can be used for a large set of measurements without any previous plating or activation. The obtained detection and quantification limits suggest that BispSPEs produce a better analytical performance as compared to In-situ BiSPCE for Pb(II) and Cd(II) determination, but also to Ex-situ BiSPCE for Cd(II) determination. The results confirm the applicability of these devices for the determination of low level concentrations of these metal ions in natural samples with very high reproducibility (0.7% and 2.5% for Pb(II) and Cd(II) respectively), and good trueness (0.3% and 2.4% for Pb(II) and Cd(II) respectively). PMID:24401424

Adsorption isotherms of NaCl on activated carbon cloth (ACC) and titania-incorporated activated carbon cloth (Ti-ACC) under an electric field were investigated to deduce the role of titania in capacitive deionization (CDI) of NaCl. Electrosorption of NaCl on the ACC was significantly increased by titania incorporation, whereas its physical adsorption was considerably decreased, resulting in an improved performance of the Ti-ACC as a CDI electrode. Langmuir isotherms based on a localized and fixed amount of adsorption were suitable for the simulation of electrosorption and physical adsorption of ions on the ACC electrodes. The variances of q(m) and b of Langmuir isotherms with electric potential indicate increases in the number of ions per adsorption site and in electrosorption strength of ions by titania incorporation. A cyclic voltammetric study for ion adsorption on ACC electrodes confirms the reversibility between electrosorption and desorption of ions, regardless of titania incorporation. PMID:16256660

This article represented the data about antioxidant activity in the red table and liqueurfaults, prepared from the types of grapes of Cabernet, Merlot and Saperavi. The antioxidant activity of faults in the conversion to TROLOX, the synthetic analog of gallic acid, was determined by voltammetric method. The determination of antioxidant activity was conducted in the young faults (through 2 month after the completion of fermentation) and through half a year the storage without the air inlet. It has been established that the value of antioxidant activity depended on the type of grapes and technology of the production of wine. It was shown that the addition of ethyl alcohol in the production of wines such as Cahors ensured an increase in the extraction of phenol connections from the skin of grapes. This lead to an increase of the antioxidant activity in the Cahors wines in the comparison with the table wine. During the storage of faults the value of antioxidant activity decreased. In the fault cahors wine it remained at the higher level. PMID:27228712

Electrogenic activity of photo-bioelectrocatalytic /photo-biological fuel cell (PhFC) was evaluated in a mixotrophic mode under anoxygenic microenvironment using photosynthetic consortia as biocatalyst. An acetate rich wastewater was used as anolyte for harnessing energy along with additional treatment. Mixotrophic operation facilitated good electrogenic activity and wastewater treatment associated with biomass growth. PhFC operation documented feasible microenvironment for the growth of photosynthetic bacteria compared to algae which was supported by pigment (total chlorophyll and bacteriochlorophyll) and diversity analysis. Pigment data also illustrated the association between bacterial and algal species. The synergistic interaction between anoxygenic and oxygenic photosynthesis was found to be suitable for PhFC operation. Light dependent deposition of electrons at electrode was relatively higher compared to dark dependent electron deposition under anoxygenic condition. PhFC documented for good volatile fatty acids removal by utilizing them as electron donor. Bioelectrochemical behavior of PhFC was evaluated by voltammetric and chronoamperometry analysis. PMID:22297047

As evidenced from the increase of electrocatalytic currents measured under voltammetric and chronoamperometric conditions, the activity of bimetallic Pt-Ru and Pt-Sn nanoparticles towards oxidation of ethanol is increased by modification of their surfaces with ultra-thin films of phosphododecamolybdic acid (H 3PMo 12O 40). The enhancement effect has been most pronounced in a case of heteropolymolybdate-modified carbon-supported Pt-Sn catalysts. Independent high-resolution XPS measurements indicate the ability of heteropolymolybdates to stabilize tin (in bimetallic Pt-Sn particles) at higher oxidation states (presumably as tin oxo species). The overall activation effect may also be ascribed to changes in the morphology of catalytic films following modification with heteropolymolybdates. Presence of the polyoxometallate is also likely to increase of the interfacial population of reactive oxo groups in the vicinity of platinum centers.

Cobalt sulfides have become promising electrode materials for lithium ion batteries while their applications in rechargeable magnesium batteries are rarely reported. In this paper, we have done some research on the electrochemical properties of cobalt sulfide (CoS) as the cathode-active material for rechargeable magnesium batteries. Flower-like CoS with nanostructures is synthesized by a facile solvothermal route. The obvious redox peaks on the cyclic voltammetric curves confirm the possibility of applications. The galvanostatic charge-discharge tests display excellent cycle stability and high coulomb efficiency. Meanwhile, the possible mechanism of charge-discharge reactions is proposed and discussed. These results show that flower-like CoS is a promising candidate as cathode-active material for rechargeable magnesium batteries.

The signal transduction and enzyme activity were investigated in biosensors based on the glucose oxidase (GOx) and carbon nanotubes (CNT) embedded in a bio-adhesive film of chitosan (CHIT). The voltammetric studies showed that, regardless of CHIT matrix, the GOx adsorbed on CNT yielding a pair of surface-confined current peaks at -0.48 V. The anodic peak did not increase in the presence of glucose in an O2-free solution indicating the lack of direct electron transfer (DET) between the enzymatically active GOx and CNT. The voltammetric peaks were due to the redox of enzyme cofactor flavin adenine dinucleotide (FAD), which was not the part of active enzyme. The presented data suggest that DET may not be happening for any type of GOx/CNT-based sensor. The biosensor was sensitive to glucose in air-equilibrated solutions indicating the O2-mediated enzymatic oxidation of glucose. The signal transduction relied on the net drop in a biosensor current that was caused by a decrease in a 4-e- O2 reduction current and an increase in a 2-e- H2O2 reduction current. The enzyme assays showed that CNT nearly doubled the retention of GOx in a biosensor while decreasing the average enzymatic activity of retained enzyme by a factor of 4-5. Such inhibition should be considered when using a protein-assisted solubilization of CNT in water for biomedical applications. The proposed analytical protocols can be also applied to study the effects of nanoparticles on proteins in assessing the health risks associated with the use of nanomaterials. PMID:24274759

We have published recently the effect of dissimilar diffusion coefficients on the size of the voltammetric waves from a mixture of two redox-active compounds. Similarly, at the potential range where three redox-active species, decamethylferrocene (dMeFc), ferrocene (Fc) and N-methylphenothiazine (MePTZ), are oxidized simultaneously with rates controlled by linear diffusion, electrogenerated radicals diffusing outwards from the electrode react with the original species diffusing towards the electrode from the bulk; thus, Fc(+) reacts with dMeFc producing Fc and dMeFc(+), while MePTZ(+) reacts both with dMeFc producing MePTZ and dMeFc(+), and with Fc producing MePTZ and Fc(+). These reactions replace dMeFc with Fc at the second plateau, and both dMeFc and Fc with MePTZ at the third plateau. Since the diffusion coefficients of the three species are not equal, the mass-transfer limited currents of the second and the third oxidation wave plateaus change by approx. 10%. Numerical simulations of the experimental voltamograms support this mechanism. Similar results were also obtained for a mixture of four redoxactive compounds. The implications of this non-additive nature of currents on: (a) the use of internal voltammetric standards for quantitative analysis of a mixture of redox-active compounds; and, (b) the half wave potentials (E1/2) of the 2nd, 3rd and 4th waves for qualitative analysis, will be discussed.

Nitrate dosing is widely used to control sulfide and methane formation in sewers. The impact of nitrate on sulfide and methane production by sewer biofilms in rising mains has been elucidated recently. However, little is known about the effect of nitrate on biologically active sewer sediment, which is substantially thicker than rising main biofilms (centimeters vs. hundreds of micrometers, respectively). In this study, we investigated the effect of nitrate addition to sewer sediment cultivated in lab-scale sewer sediment reactors. Batch test results showed that nitrate addition does not suppress sulfide production in sewer sediment, but it reduces sulfide accumulation through anoxic sulfide oxidation in the sediment and hence, also reduces sulfide accumulation in the bulk water. Microsensor measurement of sediment sulfide revealed the presence of sulfide oxidation and sulfide production zones with the interface dynamically regulated by the depth of nitrate penetration. In contrast, the methane production activity of sewer sediment was substantially reduced, likely due to the long-term inhibitory effects of nitrate on methanogens. Pore water measurements showed that methane production activity in the sediment zone with frequent nitrate exposure was completely suppressed, and consequently, the methane production zone re-established deeper in the sediment where nitrate penetration was infrequent. PMID:25727155

This review examines the electrochemical techniques used to study extracellular electron transfer in the electrochemically active biofilms that are used in microbial fuel cells and other bioelectrochemical systems. Electrochemically active biofilms are defined as biofilms that exchange electrons with conductive surfaces: electrodes. Following the electrochemical conventions, and recognizing that electrodes can be considered reactants in these bioelectrochemical processes, biofilms that deliver electrons to the biofilm electrode are called anodic, ie electrode-reducing, biofilms, while biofilms that accept electrons from the biofilm electrode are called cathodic, ie electrode-oxidizing, biofilms. How to grow these electrochemically active biofilms in bioelectrochemical systems is discussed and also the critical choices made in the experimental setup that affect the experimental results. The reactor configurations used in bioelectrochemical systems research are also described and the authors demonstrate how to use selected voltammetric techniques to study extracellular electron transfer in bioelectrochemical systems. Finally, some critical concerns with the proposed electron transfer mechanisms in bioelectrochemical systems are addressed together with the prospects of bioelectrochemical systems as energy-converting and energy-harvesting devices. PMID:22856464

This review examines the electrochemical techniques used to study extracellular electron transfer in the electrochemically active biofilms that are used in microbial fuel cells and other bioelectrochemical systems. Electrochemically active biofilms are defined as biofilms that exchange electrons with conductive surfaces: electrodes. Following the electrochemical conventions, and recognizing that electrodes can be considered reactants in these bioelectrochemical processes, biofilms that deliver electrons to the biofilm electrode are called anodic, ie electrode-reducing, biofilms, while biofilms that accept electrons from the biofilm electrode are called cathodic, ie electrode-oxidizing, biofilms. How to grow these electrochemically active biofilms in bioelec-trochemical systems is discussed and also the critical choices made in the experimental setup that affect the experimental results. The reactor configurations used in bioelectrochemical systems research are also described and the authors demonstrate how to use selected voltammetric techniques to study extracellular electron transfer in bioelectrochemical systems. Finally, some critical concerns with the proposed electron transfer mechanisms in bioelectrochemical systems are addressed together with the prospects of bioelectrochemical systems as energy-converting and energy-harvesting devices. PMID:22856464

The electrochemical response of many redox species on boron-doped diamond (BDD) electrodes can be strongly dependent on the type of chemical termination on their surface, hydrogen (HT-BDD) or oxygen (OT-BDD). For instance, on an HT-BDD electrode the [Fe(CN)6](3-/4-) redox system presents a reversible voltammetric behavior, whereas the oxidation overpotential of ascorbic acid (AA) is significantly decreased. Moreover, the electrochemical activity of BDD electrodes can be significantly affected by electrochemical pretreatments, with cathodic pretreatments (CPTs) leading to redox behaviors associated with HT-BDD. Here we report on the effect of increasingly severe CPTs on the electrochemical activity of a highly doped BDD electrode, assessed with the [Fe(CN)6](3-/4-) and AA redox probes, and on the atomic bonding structure on the BDD surface, assessed by XPS. The hydrogenation level of the BDD surface was increased by CPTs, leading to decreases of the total relative level of oxidation of the BDD surface of up to 36%. Contrary to what is commonly assumed, we show that BDD surfaces do not need to be highly hydrogenated to ensure that a reversible voltammetric behavior is obtained for Fe(CN)6](3-/4-); after a CPT, this was attained even when the total relative level of oxidation on the BDD surface was about 15%. At the same time, the overpotential for AA oxidation was confirmed as being very sensitive to the level of oxidation of the BDD surface, a behavior that might allow the use of AA as a secondary indicator of the relative atomic bonding structure on the BDD surface. PMID:27101534

We synthesized mesoporous carbon from pre-cross-linked lignin gel impregnated with a surfactant as the pore-forming agent, and then activated the carbon through physical and chemical methods to obtain activated mesoporous carbon. The activated mesoporous carbons exhibited 1.5- to 6-fold increases in porosity with a maximum BET specific surface area of 1148 m2/g and a pore volume of 1.0 cm3/g. Slow physical activation helped retain dominant mesoporosity; however, aggressive chemical activation caused some loss of the mesopore volume fraction. Plots of cyclic voltammetric data with the capacitor electrode made from these carbons showed an almost rectangular curve depicting the behavior of ideal double-layer capacitance. Although the pristine mesoporous carbon exhibited the same range of surface-area-based capacitance as that of other known carbon-based supercapacitors, activation decreased the surface-area-based specific capacitance and increased the gravimetric-specific capacitance of the mesoporous carbons. Surface activation lowered bulk density and electrical conductivity. Warburg impedance as a vertical tail in the lower frequency domain of Nyquist plots supported good supercapacitor behavior for the activated mesoporous carbons. Our work demonstrated that biomass-derived mesoporous carbon materials continue to show potential for use in specific electrochemical applications.

The temporal and spatial effects of selenite (SeO3(2-)) on the physical properties and respiratory activity of Phanerochaete chrysosporium biofilms, grown in flow-cell reactors, were investigated using oxygen microsensors and confocal laser scanning microscopy (CLSM) imaging. Exposure of the biofilm to a SeO3(2-) load of 1.67mgSeL(-1)h(-1) (10mgSeL(-1) influent concentration), for 24h, resulted in a 20% reduction of the O2 flux, followed by a ∼10% decrease in the glucose consumption rate. Long-term exposure (4days) to SeO3(2-) influenced the architecture of the biofilm by creating a more compact and dense hyphal arrangement resulting in a decrease of biofilm thickness compared to fungal biofilms grown without SeO3(2-). To the best of our knowledge, this is the first time that the effect of SeO3(2-) on the aerobic respiratory activity on fungal biofilms is described. PMID:26935326

The antioxidative mechanism of action of betalains is of significant interest because these pigments are recently emerging as highly bio-active natural compounds with potential benefits to human health. Betanidin, the basic betacyanin, comprises the 5,6-dihydroxyl moiety, which results in its high antioxidant activity. Oxidation of betanidin by voltammetric techniques and chro matographic identification of the oxidation products with spectrophotometric and mass spectrometric detection (LC-DAD-MS/MS) were performed. Two main oxidation peaks for betanidin are observable at pH 3-5. These peaks become merged at higher pH, suggesting a different mechanism of oxidation at higher and lower pH values. The low oxidation potential of betanidin confirms its very strong reduction properties. The presence of two prominent oxidized products, 2-decarboxy-2,3-dehydrobetanidin and 2,17-bidecarboxy-2,3-dehydrobetanidin, indicates their generation through two reaction routes with two different quinonoid intermediates: dopachrome derivative and quinone methide. Both lead to the decarboxylative dehydrogenation of betanidin. Subsequent oxidation and rearrangement of the conjugated chromophoric system results in formation of 14,15-dehydrogenated derivatives. PMID:21913685

The mammalian olfactory system has an exquisite capacity to rapidly recognize and discriminate thousands of distinct odors in our environment. Our research group focus on reading information from olfactory bulb circuit of anethetized Sprague-Dawley rat and utilize artificial recognition system for odor discrimination. After being stimulated by three odors with concentration of 10 μM to rat nose, the response of mitral cells in olfactory bulb is recorded by eight channel microwire sensor array. In 20 sessions with 3 animals, we obtained 30 discriminated individual cells recordings. The average firing rates of the cells are Isoamyl acetate 26 Hz, Methoxybenzene 16 Hz, and Rose essential oil 11 Hz. By spike sorting, we detect peaks and analyze the interspike interval distribution. Further more, principal component analysis is applied to reduce the dimensionality of the data sets and classify the response.

Many chemical analysis problems exist that encourage the development of small, low-cost, low power, chemical sensors in many of these applications, while speciation of the sample is unnecessary due to prior knowledge of the sample constituents, it is necessary to monitor, in near real-time, the concentration of a Particular species of interest, An example of this of problem would be the monitoring of a chemical process such as steam reforming of chemical waste or ground water monitoring where prior laboratory analysis has determined the constituents. In applications such as these, it is worthwhile to trade off the sensitivity and speciation that can be obtained by taking individual samples and analyzing them in a laboratory for the near real-time, low-cost measurements that can be achieved using a solid-state transducer. In this paper, several different types of sensor platforms and applications that require CSFs bonded to the platform will be discussed. Among these are surface acoustic wave (SAW) based sensors, optical fiber-based sensors, and Si-based sensors. Each will be described and applications will be discussed.

This article presents the design, construction and characterization of a novel type of light probe for measuring the angular radiance distribution of light fields. The differential acceptance angle (DAA) probe can resolve the directionality of a light field in environments with steep light gradients, such as microbial mats, without the need to remove, reorient, and reinsert the probe, a clear advantage over prior techniques. The probe consists of an inner irradiance sensor inside a concentric, moveable light-absorbing sheath. The radiative intensity in a specific zenith direction can be calculated by comparing the irradiance onto the sensor at different acceptance angles. We used this probe to measure the angular radiance distribution of two sample light fields, and observed good agreement with a conventional radiance probe. The DAA probe will aid researchers in understanding light transfer physics in dense microbial communities and expedite validation of numerical radiative transfer models for these environments. PMID:25763775

We present polymeric packaging methods used for subcutaneous, fully implantable, broadband, and wireless neurosensors. A new tool for accelerated testing and characterization of biocompatible polymeric packaging materials and processes is described along with specialized test units to simulate our fully implantable neurosensor components, materials and fabrication processes. A brief description of the implantable systems is presented along with their current encapsulation methods based on polydimethylsiloxane (PDMS). Results from in-vivo testing of multiple implanted neurosensors in swine and non-human primates are presented. Finally, a novel augmenting polymer thin film material to complement the currently employed PDMS is introduced. This thin layer coating material is based on the Plasma Enhanced Chemical Vapor Deposition (PECVD) process of Hexamethyldisiloxane (HMDSO) and Oxygen (O(2)). PMID:23365999

We present polymeric packaging methods used for subcutaneous, fully implantable, broadband, and wireless neurosensors. A new tool for accelerated testing and characterization of biocompatible polymeric packaging materials and processes is described along with specialized test units to simulate our fully implantable neurosensor components, materials and fabrication processes. A brief description of the implantable systems is presented along with their current encapsulation methods based on polydimethylsiloxane (PDMS). Results from in-vivo testing of multiple implanted neurosensors in swine and non-human primates are presented. Finally, a novel augmenting polymer thin film material to complement the currently employed PDMS is introduced. This thin layer coating material is based on the Plasma Enhanced Chemical Vapor Deposition (PECVD) process of Hexamethyldisiloxane (HMDSO) and Oxygen (O2). PMID:23365999

During nitrification, nitrite is produced as an intermediate when ammonia is oxidized to nitrate. It is well established that nitrifying biofilm are involved in nitrification episodes in chloraminated drinking water distribution systems with nitrite accumulation occurring during...

During nitrification, nitrite is produced as an intermediate when ammonia is oxidized to nitrate. It is well established that nitrifying biofilm are involved in nitrification episodes in chloraminated drinking water distribution systems with nitrite accumulation occurring during ...

Our overall intent in this aspect of the project were to establish a collaborative effort between several departments at Montana State University for developing advanced optoelectronic technology for advancing the state-of-the-art in optical remote sensing of the environment. Our particular focus was on development of small systems that can eventually be used in a wide variety of applications that might include ground-, air-, and space deployments, possibly in sensor networks. Specific objectives were to: 1) Build a field-deployable direct-detection lidar system for use in measurements of clouds, aerosols, fish, and vegetation; 2) Develop a breadboard prototype water vapor differential absorption lidar (DIAL) system based on highly stable, tunable diode laser technology developed previously at MSU. We accomplished both primary objectives of this project, in developing a field-deployable direct-detection lidar and a breadboard prototype of a water vapor DIAL system. Paper summarizes each of these accomplishments.

The sensing characteristics of a cermet electrochemical cell, expressed as NiO|Pt|solid electrolyte|Pt were investigated by applying cyclic voltammetry to the Pt electrodes and measuring changes in ionic current through the solid electrolyte. Features of the current-voltage response (voltammograms) appear to depend uniquely on the type of gas exposed to the cell surface and the solid electrolyte material used. The novel sensors can selectively detect O{sub 2}, CO{sub 2}, and a variety of hydrocarbons. Performance characteristics such as selectivity, sensitivity, speed of response, and temperature dependence were also reported.

With the rapid development of micro systems technology and microelectronics, smart electronic systems are emerging for the continuous surveillance of relevant parameters in the body and even for closed-loop systems with a sensor feedback to drug release systems. With respect to diabetes management, there is a critical societal need for a sensor that can be used to continuously measure a patient's blood glucose concentration twenty four hours a day on a long-term basis. In this work, thin films of "stimuli-responsive" or "smart" hydrogels were combined with microfabricated piezoresistive pressure transducers to obtain "chemomechanical sensors" that can serve as selective and versatile wireless biomedical sensors. The sensitivity of hydrogels with regard to the concentration of glucose in solutions with physiological pH, ionic strength and temperature was investigated in vitro. The response of the glucose-sensitive hydrogel was studied at different regimes of the glucose concentration change and at different temperatures. Sensor response time and accuracy with which a sensor can track gradual changes in glucose was estimated.

Electret and polymer piezoelectric films have been previously integrated into Micro Electro Mechanical System (MEMS) acoustic sensors and energy harvesters. Common techniques employed in MEMS polymer integration include corona discharge [1] and backlighted thyratron [2], followed by macro-scale assembly of the polymer into the micro device. In contrast, this paper reports a method for post-fabrication in-situ polarization of polymer films embedded within the MEMS device itself. The method utilizes microplasma discharges with self-aligned charging grids integrated within the device to charge fluoropolymer films in a fashion similar to the common corona discharge technique. This in-situ approach enables the integration of uncharged polymer films into MEMS and subsequent post-fabrication and post-packaging polarization, simultaneously enabling the formation of buried or encapsulated electrets as well as eliminating the need to restrict fabrication and packaging processes that might otherwise discharge pre-charged materials. Using the in situ approach, a microscale charging grid structure is fabricated and suspended a short distance above the polymer film. After fabrication of the charging grid, standard microfabrication steps are performed to build MEMS sensors. After completing the entire fabrication and packaging flow, the polarization process is performed. When energized by a high voltage, the sharp metal edges of the charging grid lead to high dielectric fields that ionize the air in the gap and force electric charge onto the polymer surface. This paper presents modeling and results for this in situ polarization process.

One common requirement of microbolometers fabricated on both rigid and flexible substrates is the need for vacuum packaging to eliminate the thermal conductivity of air and achieve high performance. However, vacuum packaging of microbolometers is expensive and is a limiting factor in achieving truly low-cost uncooled infrared detection. Vacuum packing of microbolometers on flexible substrates requires a novel approach unless flexibility is to be sacrificed. This paper explores the vacuum packaging of microbolometers through self-packaging. In this case, the micromachined encapsulation in a vacuum cavity is investigated through computer simulation of microbolometers in flexible polyimide films and through the encapsulation of microbolometers on rigid Si substrates with a Si3N4 shell. In this manner, self packaged uncooled microbolometers were fabricated on a Si wafer with semiconducting yttrium barium copper oxide (YBCO) as the infrared sensing material. The self-packaged structure is designed such that it can be covered with a superstrate, yielding low stress in the flexible skin sensors and better detection figures of merit. The devices have demonstrated voltage responsivities over 103 V/W, detectivities above 106 cm Hz1/2/W and temperature coefficient of resistance around -3.3% K-1. Computer simulations using CoventorWare and MEMulator have been used to determine suitable materials for the process, the optimum design of a vacuum element and a streamlined process flow.

A simple and low cost optical sensor, based on porous silicon nanotechnology, has been used to detect and quantify the presence of atrazine pesticide in water and humic acid solutions. In both cases, a well defined optical signal variation can be registered, even at low concentration as 1 ppm. The phenomenon can be ascribed to the capillary infiltration of liquid into the pores, which changes the average refractive index of the structure. Due to the resonant cavity enhanced operation of the proposed sensors, very low detection limits can be reached. PMID:15741087

Seacoast Science develops chemical sensors that use polymer-coated micromachined capacitors to measure the dielectric permittivity of an array of selectively absorbing materials. We present recent results demonstrating the sensor technology's capability to detect components in explosives and toxic industrial chemicals. These target chemicals are detected with functionalized polymers or network materials, chosen for their ability to adsorb chemicals. When exposed to vapors or gases, the permittivity of these sorbent materials changes depending on the strength of the vapor-sorbent interaction. Sensor arrays made of ten microcapacitors on a single chip have been previously shown to detect vapors of organic compounds (chemical warfare agents, industrial solvents, fuels) and inorganic gases (SO2, CO2, NO2). Two silicon microcapacitor structures were used, one with parallel electrode plates and the other with interdigitated "finger-like" electrodes. The parallel-plates were approximately 300 μm wide and separated by 750 nm. The interdigitated electrodes were approximately 400 μm long and were elevated above the substrate to provide faster vapor access. Eight to sixteen of these capacitors are fabricated on chips that are 5 x 2 mm and are packaged in less than 50 cm3 with supporting electronics and batteries, all weighing less than 500 grams. The capacitors can be individually coated with different materials creating a small electronic nose that produces different selectivity patterns in response to different chemicals. The resulting system's compact size, low-power consumption and low manufacturing costs make the technology ideal for integration into various systems for numerous applications.

Advanced microfabrication processes have been developed for producing a hermetic cover wafer with low resistance dielectrically isolated through-wafer interconnects. The feasibility of manufacturing encapsulated pressure sensors, utilizing the cover-wafer approach, has been demonstrated. Such pressure sensors represent a new generation of environmentally protected, cost effective devices. The accomplishments of Phase 1 include the following: (1) the study of conversion of single crystal silicon into porous silicon; (2) the study of conversion of porous silicon into oxide; (3) process for producing through-wafer interconnects has been established; and (4) the stresses in the cover wafer have been investigated, which enabled the fabrication of flat cover-wafers. The surface and cross-sectional morphology of the cover wafer was investigated, the hermeticity and dielectric isolation of the oxidized rings was verified, the sensors compatible with the cover-wafer approach were fabricated and tested, and a new generation of sensors designed.

A device for measuring turbulence in high-speed flows is provided which includes a micro- sensor thin-film probe. The probe is formed from a single crystal of aluminum oxide having a 14 deg half-wedge shaped portion. The tip of the half-wedge is rounded and has a thin-film sensor attached along the stagnation line. The bottom surface of the half-wedge is tilted upward to relieve shock induced disturbances created by the curved tip of the half-wedge. The sensor is applied using a microphotolithography technique.

Biofilm reactors were constructed to grow stratified multispecies biofilm in oil sands process-affected water (OSPW) supplemented with growth medium. The development of sulfate reducing bacteria (SRB) within the biofilm and the biofilm treatment of OSPW were evaluated. The community structure and potential activity of SRB in the biofilm were investigated with H2S microsensor measurements, dsrB gene-based denaturing gradient gel electrophoresis (DGGE), and the real time quantitative polymerase chain reaction (qPCR). Multispecies biofilm with a thickness of 1000 μm was successfully developed on engineered biocarriers. H2S production was observed in the deeper anoxic zone of the biofilm from around 750 μm to 1000 μm below the bulk water-biofilm interface, revealing sulfate reduction in the deeper zone of the stratified biofilm. The biofilm removed chemical oxygen demand (COD), sulfate, and nitrogen. The study expands current knowledge of biofilm treatment of OSPW and the function of anaerobic SRB in OSPW biofilm, and thus provides information for future bioreactor development in the reclamation of OSPW. PMID:26204047

SRI International (SRI) is developing ceramic-based microsensors to detect exhaust gases such as NO, NO{sub 2}, and CO in advanced combustion and gasification systems under this DOE NETL-sponsored research project. The sensors detect the electrochemical activity of the exhaust gas species on catalytic electrodes attached to a solid state electrolyte and are designed to operate at the high temperatures, elevated pressures, and corrosive environments typical of large power generation exhausts. The sensors can be easily integrated into online monitoring systems for active emission control. The ultimate objective is to develop sensors for multiple gas detection in a single package, along with data acquisition and control software and hardware, so that the information can be used for closed-loop control in novel advanced power generation systems. This report details the Phase I Proof-of-Concept, research activities performed from October 2003 to March 2005. SRI's research work includes synthesis of catalytic materials, sensor design and fabrication, software development, and demonstration of pulse voltammetric analysis of NO, NO{sub 2}, and CO gases on catalytic electrodes.

Background Continuous monitoring of glucose by implantable microfabricated devices offers key advantages over current transcutaneous glucose sensors that limit usability due to their obtrusive nature and risk of infection. A successful sensory implant should be biocompatible and retain long-lasting function. Polymorphonuclear leukocytes (PMN) play a key role in the inflammatory system by releasing enzymes, cytokines, and reactive oxygen species, typically as a response to complement activation. The aim of this study was to perform an in vitro analysis of PMN activation as a marker for biocompatibility of materials and to evaluate the role of complement in the activation of PMN. Methods Fifteen candidate materials of an implantable glucose sensor were incubated in lepirudin-anticoagulated whole blood. The cluster of differentiation molecule 11b (CD11b) expression on PMN was analyzed with flow cytometry and the myeloperoxidase (MPO) concentration in plasma was analyzed with enzyme-linked immunosorbent assay. Complement activation was prevented by the C3 inhibitor compstatin or the C5 inhibitor eculizumab. Results Three of the biomaterials (cellulose ester, polyamide reverse osmosis membrane, and polyamide thin film membrane), all belonging to the membrane group, induced a substantial and significant increase in CD11b expression and MPO release. The changes were virtually identical for these two markers. Inhibition of complement with compstatin or eculizumab reduced the CD11b expression and MPO release dose dependently and in most cases back to baseline. The other 12 materials did not induce significant PMN activation. Conclusion Three of the 15 candidate materials triggered PMN activation in a complement-dependent manner and should therefore be avoided for implementation in implantable microsensors. PMID:22226271

A simple and cost effective method for the determination of restriction endonuclease activity is presented. dsDNA immobilized at a gold electrode surface is used as the enzymatic substrate, and an external cationic redox probe is employed in voltammetric measurements for analytical signal generation. The assessment of enzyme activity is based on a decrease of a current signal derived from reduction of methylene blue which is present in the sample solution. For this reason, the covalent attachment of the label molecule is not required which significantly reduces costs of the analysis and simplifies the entire determination procedure. The influence of buffer components on utilized dsDNA/MCH monolayer stability and integrity is also verified. Electrochemical impedance spectroscopy measurements reveal that due to pinhole formation during enzyme activity measurement the presence of any surfactants should be avoided. Additionally, it is shown that the sensitivity of the electrochemical biosensor can be tuned by changing the restriction site location along the DNA length. Under optimal conditions the proposed biosensor exhibits a linear response toward PvuII activity within a range from 0.25 to 1.50 U/μL. PMID:26859430

In the present paper, a new bisphosphoramidate derivative compound, 1, 4-bis(N-methyl)-benzene-bis(N-phenyl, N-benzoylphosphoramidate) (BMBPBP), was synthesized and used as a mediator for the electrocatalytic oxidation of olanzapine. The electro-oxidation of olanzapine at the surface of the BMBPBP/CdS-quantum dots/multi-walled carbon nanotubes (BMBPBP/CdS-QDs/MWCNTs) modified gold electrode was studied using cyclic voltammetry, chronoamperometry and electrochemical impedance spectroscopy. This sensor showed an excellent electrocatalytic oxidation activity toward olanzapine at less positive potential, pronounced current response, and good sensitivity. The diffusion coefficient and kinetic parameters (such as electron transfer coefficient and the heterogeneous rate constant) were determined for olanzapine oxidation, using the electrochemical approaches. Surface morphology and electrochemical properties of the prepared modified electrode were investigated by scanning electron microscopy (SEM), cyclic voltammetry and electrochemical impedance spectroscopy techniques. The hydrodynamic amperometry at rotating modified electrode at constant potential versus reference electrode was used for detection of olanzapine. Under optimized conditions, the calibration plot was linear in the concentration range of 20 nM to 100 μM and detection limit was found to be 6 nM. The proposed method was successfully applied to the determination of olanzapine in pharmaceuticals and human serum samples. PMID:26706508

We report a comparative study of the alloy formation and electrochemical activity of dealloyed PtCo 3 and PtCu 3 nanoparticle electrocatalysts for the oxygen reduction reaction (ORR). For the Pt-Co system the maximum annealing temperatures were 650 °C, 800 °C and 900 °C for 7 h to drive the Pt-Co alloy formation and the particle growth. EDS and XRD were employed for the characterization of catalyst powders. The RDE and RRDE experiments were conducted in 0.1 M HClO 4 at room temperature. We demonstrate that the mass and surface area specific ORR activities of Pt-Co and Pt-Cu alloys after voltammetricactivation exhibit a considerable improvement compared to those of pure Pt/C. The dealloyed PtCo 3 (800 °C/7 h) electrocatalyst performs 3 times higher in terms of Pt-based mass activity and 4-5 times higher in terms of ECSA-based specific activity than a 28.2 wt.% Pt/C. Dealloyed Pt-Co catalysts (800 °C/7 h) show the most favorable balance between mass and specific ORR activity with a particle size of 2.2 ± 0.1 nm. We hypothesize that geometric strain effects of the dealloyed Pt-Co nanoparticles, similar to those found in dealloyed PtCu 3 nanoparticles, are responsible for the improvement in ORR activity [1].

To clearly illustrate the antibacterial activity of graphene on anodic exoelectrogen, the growth of a Shewanella oneidensis MR-1 biofilm on graphene-modified anodes (GMAs) and bare graphite anodes (BGs) were compared. The GMAs with different amounts of graphene were obtained by the cyclic voltammetric electrodeposition of 5, 20 and 40 potential cycles (5-G, 20-G and 40-G). Confocal scanning laser microscopy and cyclic voltammetry results demonstrated that graphene exhibited an obvious antibacterial effect for initial Shewanella MR biofilm growth. After 5 h of inoculation, 40-G, 20-G and 5-G had 6.3, 8.8 and 13.9% lower levels of biofilm viability, respectively, compared to BG, and all three exhibited approximately 70% lower electrochemical activity compared to BG. However, 18 h later, the biofilm on the GMAs exhibited much higher viability than that of the BG, and the electrochemical activity increased to a similar level. This study revealed the dual effect of graphene, including the antibacterial activity on biofilms and the enhancement of bacterial attachment and electron transfer.

The microbial community structure and activity dynamics of a phosphate-removing biofilm from a sequencing batch biofilm reactor were investigated with special focus on the nitrifying community. O2, NO2−, and NO3− profiles in the biofilm were measured with microsensors at various times during the nonaerated-aerated reactor cycle. In the aeration period, nitrification was oxygen limited and restricted to the first 200 μm at the biofilm surface. Additionally, a delayed onset of nitrification after the start of the aeration was observed. Nitrate accumulating in the biofilm in this period was denitrified during the nonaeration period of the next reactor cycle. Fluorescence in situ hybridization (FISH) revealed three distinct ammonia-oxidizing populations, related to the Nitrosomonas europaea, Nitrosomonas oligotropha, and Nitrosomonas communis lineages. This was confirmed by analysis of the genes coding for 16S rRNA and for ammonia monooxygenase (amoA). Based upon these results, a new 16S rRNA-targeted oligonucleotide probe specific for the Nitrosomonas oligotropha lineage was designed. FISH analysis revealed that the first 100 μm at the biofilm surface was dominated by members of the N. europaea and the N. oligotropha lineages, with a minor fraction related to N. communis. In deeper biofilm layers, exclusively members of the N. oligotropha lineage were found. This separation in space and a potential separation of activities in time are suggested as mechanisms that allow coexistence of the different ammonia-oxidizing populations. Nitrite-oxidizing bacteria belonged exclusively to the genus Nitrospira and could be assigned to a 16S rRNA sequence cluster also found in other sequencing batch systems. PMID:11229931

The gut microbiota of termites and cockroaches represents complex metabolic networks of many diverse microbial populations. The distinct microenvironmental conditions within the gut and possible interactions among the microorganisms make it essential to investigate how far the metabolic properties of pure cultures reflect their activities in their natural environment. We established the cockroach Shelfordella lateralis as a gnotobiotic model and inoculated germfree nymphs with two bacterial strains isolated from the guts of conventional cockroaches. Fluorescence microscopy revealed that both strains specifically colonized the germfree hindgut. In diassociated cockroaches, the facultatively anaerobic strain EbSL (a new species of Enterobacteriaceae) always outnumbered the obligately anaerobic strain FuSL (a close relative of Fusobacterium varium), irrespective of the sequence of inoculation, which showed that precolonization by facultatively anaerobic bacteria does not necessarily favor colonization by obligate anaerobes. Comparison of the fermentation products of the cultures formed in vitro with those accumulated in situ indicated that the gut environment strongly affected the metabolic activities of both strains. The pure cultures formed the typical products of mixed-acid or butyrate fermentation, whereas the guts of gnotobiotic cockroaches accumulated mostly lactate and acetate. Similar shifts toward more-oxidized products were observed when the pure cultures were exposed to oxygen, which corroborated the strong effects of oxygen on the metabolic fluxes previously observed in termite guts. Oxygen microsensor profiles of the guts of germfree, gnotobiotic, and conventional cockroaches indicated that both gut tissue and microbiota contribute to oxygen consumption and suggest that the oxygen status influences the colonization success. PMID:26637604

The gut microbiota of termites and cockroaches represents complex metabolic networks of many diverse microbial populations. The distinct microenvironmental conditions within the gut and possible interactions among the microorganisms make it essential to investigate how far the metabolic properties of pure cultures reflect their activities in their natural environment. We established the cockroach Shelfordella lateralis as a gnotobiotic model and inoculated germfree nymphs with two bacterial strains isolated from the guts of conventional cockroaches. Fluorescence microscopy revealed that both strains specifically colonized the germfree hindgut. In diassociated cockroaches, the facultatively anaerobic strain EbSL (a new species of Enterobacteriaceae) always outnumbered the obligately anaerobic strain FuSL (a close relative of Fusobacterium varium), irrespective of the sequence of inoculation, which showed that precolonization by facultatively anaerobic bacteria does not necessarily favor colonization by obligate anaerobes. Comparison of the fermentation products of the cultures formed in vitro with those accumulated in situ indicated that the gut environment strongly affected the metabolic activities of both strains. The pure cultures formed the typical products of mixed-acid or butyrate fermentation, whereas the guts of gnotobiotic cockroaches accumulated mostly lactate and acetate. Similar shifts toward more-oxidized products were observed when the pure cultures were exposed to oxygen, which corroborated the strong effects of oxygen on the metabolic fluxes previously observed in termite guts. Oxygen microsensor profiles of the guts of germfree, gnotobiotic, and conventional cockroaches indicated that both gut tissue and microbiota contribute to oxygen consumption and suggest that the oxygen status influences the colonization success. PMID:26637604

Antioxidant activity of a number of small (low molecular weight) natural compounds found in spices, condiments or drugs (gallic acid, sesamol, eugenol, thymol, carvacrol, vanillin, salicylaldehyde, limonene, geraniol, 4-hexylresorcinol, etc.) has been evaluated using electrochemical and DPPH• radical scavenging measurements. Structural analysis of the tested compound suggest a remarkable activity for phenol derivatives and the importance of the -R groups located on the phenolic ring in the molecule's ability to act as free radical scavenging as well as their influence in the electrochemical behavior. The voltammetric method can be used for the determination of the antioxidant capability in the same manner as the DPPH• radical scavenging because of the correlation found between oxidation potentials and anti-radical power (ARP = 1/EC₅₀). Such electrochemical determination is fast and cheap and allows making measurements under a variety of experimental conditions. The accuracy of the electrochemical measurements is the same for all the compounds, irrespective of their scavenging activity, the opposite of what occurs in the DPPH• test. PMID:22555300

Oxovanadium (IV) complexes (1)-(3) have been synthesized by treating 2-thiophene carboxylic acid hydrazide with VOSO4⋅xH2O and VCl3(THF)3 in different M/L ratios. These complexes have been characterized by elemental analysis, UV-vis, FT-IR and mass spectrometry. The FT-IR data predicts the bidentate nature of the ligand which is also confirmed by semi-empirical study. Mass spectrometric data shows that molecular ion peak is only observed for 2-thiophene carboxylic acid hydrazide. The ESP map and thermodynamic parameters shows the presence of partial charge on atoms and stability of synthesized oxovanadium complexes, respectively. DNA binding study of complexes (1)-(3) was carried out by UV-vis and cyclic voltammetric methods which suggests the intercalative binding mode of the complexes with DNA. Cytotoxicity was checked by brine shrimp lethality assay and complex (1) showed greater cytotoxicity towards Artemia salina as compared to free ligand. Immuno-modulatory activity data shows that hydrazide ligand was more active as compared to oxovanadium complexes and standard drug. Complex (2) shows significant urease inhibition activity. The ligand and synthesized complexes were found inactive against all tested bacterial and fungal strains. PMID:24844618

This paper presents the use of square wave voltammetry (SWV) and square wave adsorptive stripping voltammetry (SWAdSV) in conjunction with a cyclic renewable silver amalgam film electrode (Hg(Ag)FE) for the determination of aclonifen in spiked water samples. A reduction peak at -0.65 V versus Ag/AgCl was obtained in the selected buffer (borax buffer with pH 9.2), exhibiting the characteristics of an irreversible reaction. The effect of square wave (SW) frequency, SW amplitude and step potential, as well as accumulation parameters (time and potential) were studied to select the optimal experimental conditions. The calibration curve was linear in the aclonifen concentration range from 1.0×10(-7) to 1.0×10(-6) mol L(-1) and from 1.0×10(-8) to1.0×10(-7) mol L(-1) for SWV and SWAdSV, respectively. The detection and quantification limits were found to be 3.1×10(-8) mol L(-1); 1.0×10(-7) mol L(-1) and 2.9×10(-9) mol L(-1); 9.6×10(-9) mol L-1 for SWV and SWAdSV, respectively. The proposed method was applied successfully in the determination of aclonifen in spiked water samples. The developed procedure can be adequate at least for screening purposes, where positive results should be confirmed by more selective method. PMID:26970782

The formation and stripping of palladium oxides on a palladium electrode in a 0.1M LiOH solution was studied by cyclic voltammetry. Cyclic polarization methods were used to form palladium oxides on the surface of the palladium electrode. Three different types of palladium oxides were found to be formed in alkaline solutions. A higher oxidation state of palladium oxide (PdO[sub 3]) can be formed (induced) on the surface of the electrode even at low anodic potential limit, 0.6 V (vs. SCE). Strong evidence that PdO[sub 3] can only be formed in a specific potential range is presented. From the voltammograms obtained after a long cyclic polarization time, the peak in the range of [minus]0.47 to [minus]0.60 V could be attributed to the reduction of dehydrated PdO.

The use of anodic stripping voltammetry (ASV) and differential pulse polarography (DPP) for the measurement of the concentrations of aquo ions in the presence of fulvic acid, and the subsequent use of these data for estimation of the metal--fulvic acid conditional stability const...

A simple, sensitive, and rapid detection of glutathione by cyclic voltammetry using a bare glassy carbon electrode is reported in which glutathione forms a 1 : 1 complex compound with copper(ii) ions. This complex compound is adsorbed onto the electrode surface and undergoes electrochemical oxidation at a characteristic oxidation potential of ca. -0.20 V vs. the standard mercury/mercurous sulphate reference electrode, which is used to detect the glutathione concentration. The linear dynamic range is obtained for a glutathione concentration from 1 μM to 12.5 μM, and the sensitivity is found to be 0.1 ± 0.002 μA μM(-1). A low limit of detection (n = 3) of 0.14 μM and a precision of 1.8% are achieved using a simple, unmodified electrode. The robustness of the present methodology is demonstrated by the successful quantitative analysis of glutathione in the presence of cysteine. PMID:27074944

An electrochemical aptasensor is a compact analytical device where the bioreceptor (aptamer) is coupled to a transducer surface to convert a biological interaction into a measurable signal (current) that can be easily processed, recorded and displayed. Since the discovery of the Systematic Evolution of Ligands by Enrichment (SELEX) methodology, the selection of aptamers and their application as bioreceptors has become a promising tool in the design of electrochemical aptasensors. Aptamers present several advantages that highlight their usefulness as bioreceptors such as chemical stability, cost effectiveness and ease of modification towards detection and immobilization at different transducer surfaces. In this review, a special emphasis is given to the potential use of electrochemical aptasensors for the detection of protein disease biomarkers using voltammetry techniques. Methods for the immobilization of aptamers onto electrode surfaces are discussed, as well as different electrochemical strategies that can be used for the design of aptasensors. PMID:27235188

Determination of the speciation of arsenic in groundwaters, using cathodic stripping voltammetry (CSV), is severely hampered by high levels of iron and manganese. Experiments showed that the interference is eliminated by addition of EDTA, making it possible to determine the arsenic speciation on-site by CSV. This work presents the CSV method to determine As(III) in high-iron or -manganese groundwaters in the field with only minor sample treatment. The method was field-tested in West-Bengal (India) on a series of groundwater samples. Total arsenic was subsequently determined after acidification to pH 1 by anodic stripping voltammetry (ASV). Comparative measurements by ICP-MS as reference method for total As, and by HPLC for its speciation, were used to corroborate the field data in stored samples. Most of the arsenic (78±0.02%) was found to occur as inorganic As(III) in the freshly collected waters, in accordance with previous studies. The data shows that the modified on-site CSV method for As(III) is a good measure of water contamination with As. The EDTA was also found to be effective in stabilising the arsenic speciation for longterm sample storage at room temperature. Without sample preservation, in water exposed to air and sunlight, the As(III) was found to become oxidised to As(V), and Fe(II) oxidised to Fe(III), removing the As(V) by adsorption on precipitating Fe(III)-hydroxides within a few hours. PMID:21807202

Three new tridentate copper(II) complexes [Cu(dthp)Cl(2)] (1) (dthp=2,6-di(thiazol-2-yl)pyridine), [Cu(dmtp)Cl(2)] (2) (dmtp=2,6-di(5-methyl-4H-1,2,4-triazol-3-yl)pyridine) and [Cu(dtp)Cl(2)] (3) (dtp=2,6-di(4H-1,2,4-triazol-3-yl)pyridine) have been synthesized and characterized. Crystal structure of complex 1 shows that the complex existed as distorted square pyramid with five co-ordination sites occupied by the tridentate ligand and the two chlorine anions. Ethidium bromide displacement assay, viscosity measurements, circular dichroism studies and cyclic voltammetric experiments suggested that these complexes bound to DNA via an intercalative mode. Three Cu(II) complexes were found to efficiently cleave DNA in the presence of sodium ascorbate, and singlet oxygen ((1)O(2)) and hydrogen peroxide were proved to contribute to the DNA cleavage process. They exhibited anticancer activity against HeLa, Hep-G2 and BEL-7402 cell lines. Nuclear chromatin cleavage has also been observed with AO/EB staining assay and the alkaline single-cell gel electrophoresis (comet assay). The results demonstrated that three Cu(II) complexes cause DNA damage that can induce the apoptosis of BEL-7402 cells. PMID:23186647

Dimerization and antioxidant activity of morin in the Triton X-100 micelles were studied by electronic absorption, ATR-FTIR spectra, cyclic voltammetric, DSC, freeze-fracture TEM, molecular modeling and ab initio quantum calculations. Morin can be solubilized in the Triton X-100 micelles and show selective dimerization in Triton X-100 micelles with different structures. In Triton X-100 spherical micelles, morin always exists in the form of dimer, and in Triton X-100 rodlike micelles, it is always in the form of monomer. The solubilization of morin dimer in Triton X-100 spherical micelles changes the micelle morphology from spherical to cubelike, and the size of the single micelle is also increased, while morin monomer links the Triton X-100 rodlike micelles and forms a kind of network micelle structure with the size of the "rod" unchanged. Solubilized and concentrated in Triton X-100 micelles, morin can protect human serum albumin from the damage induced by hydroxyl radicals effectively and even can form a kind of protein complex with human serum albumin showing more thermal stability. PMID:18510337

Double zwitterionic amino acid Schiff base, o-vanillylidene-L-histidine (OVHIS) and its copper complex (CuOVHIS) have been synthesized and characterized. CuOVHIS has distorted octahedral geometry, and OVHIS coordinates the copper ion in a tetradentate manner (N2O2). The pKa of OVHIS in aqueous solution was studied by potentiometric and spectrophotometric methods. DNA binding behavior of the compounds was investigated using spectrophotometric, cyclic voltammetric, and viscosity methods. The efficacy of DNA cleaving nature was tested on pUC19 DNA. The in vitro biological activity was tested against various micro organisms. The effect of CuOVHIS on the surface feature of Escherichia coli was analyzed by SEM. DPPH assay studies revealed that CuOVHIS has higher antioxidant activity. OVHIS inhibits proliferation of HCT117 cells with half maximal inhibition (IC50) of 71.15 ± 0.67. Chelation of OVHIS with Cu(II) ion enhances the inhibition of proliferation action (IC50 = 53.14 ± 0.67).

In this work, supergravity fields are performed to prepare Ni-CNTs composite cathodes with wool-ball-like morphology from the Watts bath containing well-distributed functionalized CNTs. The prepared Ni-CNTs composite cathodes are used as noble metal-free electrocatalyst with favorable electrocatalytic activity for hydrogen evolution reaction (HER) in alkaline solutions. The crystal structure and morphology of the composite cathodes are characterized by XRD and SEM measurements. The electrochemical activities of the cathodes are characterized through Tafel polarization measurement, electrochemical impedance spectroscopy and cyclic voltammetric study in 1.0 M NaOH solution. The results indicate that catalytic activities of the Ni-CNTs cathodes prepared under supergravity fields are enhanced significantly, and the sample prepared at rotating speed 3000 rpm from the bath containing 1 g dm-3 CNTs exhibits the highest HER activity with smallest Tafel slope and largest exchange current density of 823.9 μA cm-2. Furthermore, the effects of both the CNTs concentrations and the intensities of supergravity fields on the properties of the Ni-CNTs cathodes are investigated.

We report on new insights into the relationships between structure and activity of glassy carbon (GC), as a model material for electrocatalyst support, during its anodization in acid solution. Our investigation strongly confirms the role of CFGs in promotion of Pt activity by the "spill-over" effect related to CO(ads) for methanol electrooxidation (MEO) on a carbon-supported Pt catalyst. Combined analysis of voltammetric and impedance behaviour as well as changes in GC surface morphology induced by intensification of anodizing conditions reveal an intrinsic influence of the carbon functionalization and the structure of a graphene oxide (GO) layer on the electrical and electrocatalytic properties of activated GC. Although GO continuously grows during anodization, it structurally changes from being a graphite inter-layer within graphite ribbons toward a continuous GO surface layer that deteriorates the native structure of GC. As a consequence of the increased distance between GO-spaced graphite layers, the GC conductivity decreases until the case of profound GO exfoliation under drastic anodizing conditions. This exposes the native, yet abundantly functionalized, GC texture. While GC capacitance continuously increases with intensification of anodizing conditions, the surface nano-roughness and GO resistance reach the highest values at modest anodizing conditions, and then decrease upon drastic anodization due to the onset of GO exfoliation. We found for the first time that the activity of a GC-supported Pt catalyst in MEO, as one of the promising half-reactions in polymer electrolyte fuel cells, strictly follows the changes in GC nano-roughness and GO-induced GC resistance. The highest GC/Pt MEO activity is reached when optimal distance between graphite layers and optimal degree of GC functionalization bring the highest amount of CFGs into intimate contact with the Pt surface. This confirms the promoting role of CFGs in MEO catalysis. PMID:22648036

Six new bioactive ferrocene based phenylguanidines were successively synthesized and characterized by means of various analytical techniques like elemental analysis, FT-IR, multinuclear (1H and 13C) NMR, UV-Vis spectroscopy and cyclic voltammetry. The interaction of compounds with DNA was investigated by spectroscopic and cyclic voltammetric measurements. The interaction was found to be the electrostatic and the binding constants values were impressively larger. Compounds f-1, f-2, f-3 have slight larger binding constant values ranging from 0.8 × 105 to 2.4 × 105 as compared to g-1, g-2 and g-3 ranging from 7.6 × 104 to 1.1 × 105 which is most probably due to the presence of ferrocene at para position where the delocalization of electrons is maximum. Antioxidant activity was determined by UV-Vis spectrophotometer by using DPPH as a free radical. All the compounds exhibit good antioxidant activity and the results so obtained support the structure activity relationship.

An operational amplifier-type active filter in which the only capacitor in the circuit is the compensating capacitance of the operational amplifiers, the various feedback and coupling elements being essentially solely resistive.

In recent years, scanning electrochemical microscopy (SECM) has become an important tool in topography and activity studies on single live cells. The used analytical probes ("SECM tips") are voltammetric micro- or nanoelectrodes. The tips may be tracked across a live cell in constant-height or constant-distance mode, while kept at potentials that enable tracing of the spatiotemporal dynamics of functional chemical species in the immediate environment. Depending on the type of single live cells studied, cellular processes addressable by SECM range from the membrane transport of metabolites to the stimulated release of hormones and neurotransmitters and processes such as cell respiration or cell death and differentiation. In this chapter, we provide the key practical details of the constant-distance mode of SECM, explaining the establishment, and operation of the tailored distance control unit that maintains a stable tip-to-cell separation during scanning. The continuously maintained tip positioning of the system takes advantage of the decreasing impact of very short-range hydrodynamic tip-to-surface shear-forces on the vibrational amplitude of an oscillating SECM tip, as the input for a computer-controlled feedback loop regulation. Suitable microelectrode probes that are nondestructive to soft cells are a prerequisite for the success of this methodology and their fabrication and successful application are the other topics covered. PMID:22264538

The Um Alhool area in Qatar is a dynamic evaporative ecosystem that receives seawater from below as it is surrounded by sand dunes. We investigated the chemical composition, the microbial activity and biodiversity of the four main layers (L1-L4) in the photosynthetic mats. Chlorophyll a (Chl a) concentration and distribution (measured by HPLC and hyperspectral imaging, respectively), the phycocyanin distribution (scanned with hyperspectral imaging), oxygenic photosynthesis (determined by microsensor), and the abundance of photosynthetic microorganisms (from 16S and 18S rRNA sequencing) decreased with depth in the euphotic layer (L1). Incident irradiance exponentially attenuated in the same zone reaching 1% at 1.7-mm depth. Proteobacteria dominated all layers of the mat (24%-42% of the identified bacteria). Anoxygenic photosynthetic bacteria (dominated by Chloroflexus) were most abundant in the third red layer of the mat (L3), evidenced by the spectral signature of Bacteriochlorophyll as well as by sequencing. The deep, black layer (L4) was dominated by sulfate reducing bacteria belonging to the Deltaproteobacteria, which were responsible for high sulfate reduction rates (measured using 35S tracer). Members of Halobacteria were the dominant Archaea in all layers of the mat (92%-97%), whereas Nematodes were the main Eukaryotes (up to 87%). Primary productivity rates of Um Alhool mat were similar to those of other hypersaline microbial mats. However, sulfate reduction rates were relatively low, indicating that oxygenic respiration contributes more to organic material degradation than sulfate reduction, because of bioturbation. Although Um Alhool hypersaline mat is a nutrient-limited ecosystem, it is interestingly dynamic and phylogenetically highly diverse. All its components work in a highly efficient and synchronized way to compensate for the lack of nutrient supply provided during regular inundation periods. PMID:24658360

The Um Alhool area in Qatar is a dynamic evaporative ecosystem that receives seawater from below as it is surrounded by sand dunes. We investigated the chemical composition, the microbial activity and biodiversity of the four main layers (L1–L4) in the photosynthetic mats. Chlorophyll a (Chl a) concentration and distribution (measured by HPLC and hyperspectral imaging, respectively), the phycocyanin distribution (scanned with hyperspectral imaging), oxygenic photosynthesis (determined by microsensor), and the abundance of photosynthetic microorganisms (from 16S and 18S rRNA sequencing) decreased with depth in the euphotic layer (L1). Incident irradiance exponentially attenuated in the same zone reaching 1% at 1.7-mm depth. Proteobacteria dominated all layers of the mat (24%–42% of the identified bacteria). Anoxygenic photosynthetic bacteria (dominated by Chloroflexus) were most abundant in the third red layer of the mat (L3), evidenced by the spectral signature of Bacteriochlorophyll as well as by sequencing. The deep, black layer (L4) was dominated by sulfate reducing bacteria belonging to the Deltaproteobacteria, which were responsible for high sulfate reduction rates (measured using 35S tracer). Members of Halobacteria were the dominant Archaea in all layers of the mat (92%–97%), whereas Nematodes were the main Eukaryotes (up to 87%). Primary productivity rates of Um Alhool mat were similar to those of other hypersaline microbial mats. However, sulfate reduction rates were relatively low, indicating that oxygenic respiration contributes more to organic material degradation than sulfate reduction, because of bioturbation. Although Um Alhool hypersaline mat is a nutrient-limited ecosystem, it is interestingly dynamic and phylogenetically highly diverse. All its components work in a highly efficient and synchronized way to compensate for the lack of nutrient supply provided during regular inundation periods. PMID:24658360

A high density polyethylene (HDPE)/calcium carbonate (CaCO(3)) film containing TiO(2) was prepared via blown film extrusion process. The photocatalytic properties of this film were evaluated by voltammetric, UV-Vis spectrophotometric and gas chromatographic measurements following the decomposition rate of suitably selected molecular probes, such as 4-hydroxybenzoic acid and methylene blue. The film containing 1% w/w of TiO(2) displayed a profitable and reproducible photoinduced degradation activity towards target organic compounds. The effect of packaging photocatalytic activity on the structural and microbiological stability of a short-ripened cheese was studied. Cheese structure was assessed by dynamic, small deformation rheological tests. A container consisting of a multilayer material, where the layer brought in contact with the food, made from the HDPE+CaCO(3)+TiO(2) composite matrix, was able to provide a greater maintenance of the original cheese structure than a rigid container currently used, mainly due to the inhibition of lactic acid bacteria and coliforms. PMID:23411292

The mononuclear copper(II) complexes (1&2) of ligands L1 [N,N";-bis(2-hydroxy-5-methylbenzyl)-1,4-bis(3-iminopropyl)piperazine] or L2 [N,N";-bis(2-hydroxy-5-bromobenzyl)-1,4-bis(3-iminopropyl) piperazine] have been synthesized and characterised. The single crystal X-ray study had shown that ligands L1 and L2 crystallize in a monoclinic crystal system with P21/c space group. The mononuclear copper(II) complexes show one quasireversible cyclic voltammetric response near cathodic region (-0.77 to -0.85 V) in DMF assignable to the Cu(II)/Cu(I) couple. Binding interaction of the complexes with calf thymus DNA (CT DNA) investigated by absorption studies and fluorescence spectral studies show good binding affinity to CT DNA, which imply both the copper(II) complexes can strongly interact with DNA efficiently. The copper(II) complexes showed efficient oxidative cleavage of plasmid pBR322 DNA in the presence of 3-mercaptopropionic acid as reducing agent through a mechanistic pathway involving formation of singlet oxygen as the reactive species. The Schiff bases and their Cu(II) complexes have been screened for antibacterial activities which indicates that the complexes exhibited higher antimicrobial activity than the free ligands.

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Dendrimers are self-repeating globular branched star molecules, whose fractal structure continues to fascinate, challenge, and inspire. Functional dendrimers may incorporate redox centers, and potential applications include antennae molecules for light harvesting, sensors, mediators, and artificial biomolecules. We report the synthesis and redox properties of four star systems incorporating the 4-benzoyl-N-alkylpyridinium cation; the redox potential varies along the branches but remains constant at fixed radii. Bulk electrolysis shows that at a semi-infinite time scale all redox centers are electrochemically accessible. However, voltammetric analysis (cyclic voltammetry and differential pulse voltammetry) shows that on1y two of the three redox-active centers in the perimeter are electrochemically accessible during potential sweeps as slow as 20 mV/s and as fast as 10 V/s. On the contrary, both redox centers along branches are accessible electrochemically within the same time frame. These results are explained in terms of slow through-space charge transfer and the globular 3-D folding of the molecules and are discussed in terms of their implications on the design of efficient redox functional dendrimers.

Composite electrocatalytic materials that utilize carbon (Vulcan) supported Pt or PtRu nanoparticles dispersed within thin films of zirconia (ZrO2) are considered here for oxidation of such a biofuel as ethanol in acid medium. The systems were characterized using electrochemical techniques as well as transmission electron microscopy. The enhancement of activity was clearly evident upon comparison of the respective voltammetric and chronoamperometric current densities recorded (at room temperature in 0.5 mol dm-3H2SO4 containing 0.5 mol dm-3 ethanol) using the Vulcan supported Pt and PtRu catalysts in the presence and absence of zirconia. In all cases, the noble metal loading was the same, 100 μg cm-2. Apparently, the existence of large population of hydroxyl groups (originating from zirconia) in the vicinity of Pt-based catalyst, in addition to possible specific interactions between zirconia and the ruthenium component of PtRu, facilitated the oxidative removal (from Pt) of the passivating (e.g., CO) reaction intermediates (adsorbates). By utilizing carbon supported, rather than bare or unsupported, Pt or PtRu nanoparticles (dispersed within the semiconducting zirconia), the overall charge distribution at the electrocatalytic interface was improved.

The complexes with general formula cis-(CO)-trans-(X)-[Ru(CO)2(HL)X2] (where X = Cl (1) and I (2)) have been synthesized by the reaction of 3-(2-(methylthio) phenylazo)-4-hydroxy-3-penten-2-one (HL) with ruthenium carbonyls, [Ru(CO)2Cl2]n/[Ru(CO)4I2]. The proposed geometry of the complexes has been supported by elemental and mass analysis abetted with several spectroscopic techniques. The complexes exhibit a quasi-reversible one electron Ru(II)/Ru(III) oxidation couple at 0.88-1.12 V along with ligand based reduction in cyclic voltammetric study. The electronic structure of the complexes has been explained by quantum mechanical calculations by DFT/B3LYP method. Catalytic activities of the compounds are investigated by the oxidation of primary and secondary alcohols to the respective aldehydes and ketones with moderate to high conversions in presence of N-methylmorpholine-N-oxide (NMO) as co-oxidant.

Electronic components and micro-sensors utilize ceramic substrates, copper and aluminum interconnect and silicon. The joining of these combinations require pre-metallization such that solders with fluxes can wet such combinations of metals and ceramics. The paper will present a new solder alloy that can bond metals, ceramics and composites. The alloy directly wets and bonds in air without the use flux or premetallized layers. The paper will present typical processing steps and joint microstructures in copper, aluminum, aluminum oxide, aluminum nitride, and silicon joints.

A method of detecting an activator, the method including impinging with an activator a receptor material lacking a photoluminescent material and generating a by-product of a radioactive decay due to the activator impinging the reeptor material. The method further including, generating light from the by-product via the Cherenkov effect and identifying a characteristic of the activator based on the light.

Tungsten trioxide, unhydrated with hexagonal structure (h-WO 3), has been prepared by hydrothermal method at a temperature of 180 °C in acidified sodium tungstate solution. Thus prepared h-WO 3 has been characterized by X-ray diffraction (XRD) method and using electrochemical techniques. The morphology has been examined by scanning and transmission electron microscopies (SEM and TEM) and it is consistent with existence of nanorods of 50-70 nm diameter and up to 5 μm length. Cyclic voltammetric characterization of thin films of h-WO 3 nanorods has revealed reversible redox behaviour with charge-discharge cycling corresponding to the reversible lithium intercalation/deintercalation into the crystal lattice of the h-WO 3 nanorods. In propylene carbonate containing LiClO 4, two successive redox processes of hexagonal WO 3 nanorods are observed at the scan rate of 50 mV/s. Such behaviour shall be attributed to the presence of at least two W atoms of different surroundings in the lattice structure of h-WO 3 nanorods. On the other hand, in aqueous LiClO 4 solution, only one redox process is observed at the scan rate of 10 mV/s. The above observations can be explained in terms of differences in the diffusion of ions inside two types of channel cavities existing in the structure of the h-WO 3 nanorods. Moreover, the material can be applied as active support for the catalytic bi-metallic Pt-Ru nanoparticles during electrooxidation of ethanol in acid medium (0.5 mol dm -3 H 2SO 4).

Dense, active systems show active turbulence, a state characterised by flow fields that are chaotic, with continually changing velocity jets and swirls. Here we review our current understanding of active turbulence. The development is primarily based on the theory and simulations of active liquid crystals, but with accompanying summaries of related literature.

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The electrochemical single-cell analysis for enzyme activity was developed using microcells on a microcell array coupled with a positionable dual microelectrode. The microcell array with the nanoliter-scale microcells was constructed using simple chemical etching without photolithographic techniques. The positionable dual microelectrodes consisted of the nanometer-to-micrometer-radius Au disk working electrode and a approximately 80-microm-radius Ag/AgCl reference electrode. Peroxidase was chosen as the model enzyme. Factors that concern electrochemical single-cell analysis in microcells such as solution evaporation, interference of soluble oxygen, electrode size, solution volume, and electrode fouling were investigated and discussed. The 20 or 100 nL of detection volume was found to be suitable for peroxidase determination in single neutrophils or single acute promyelocytic leukemia cells without interference from intracellular macromolecules and electrode fouling, when the dual electrode with a 10-microm-radius Au disk working electrode was used. Cells were perforated with digitonin before transferring them into the microcells, to lyse cells easily. The perforated cells were transferred into the microcells by pushing a microscope slide on a drop of the cell suspension on the microcell array. After a single cell in the microcell was lysed using a freeze-thawing technique and allowed to dry, physiological buffer saline containing 2.0 x 10(-3) mol/L hydroquinone and 2.0 x 10(-3) mol/L H2O2 as the substrates of the enzyme-catalyzed reaction was added. The microcell array was positioned in a constant-humidity chamber to prevent evaporation. Then the dual electrode was inserted into the microcell by means of a scanning electrochemical microscope and the product benzoquinone of the enzyme-catalyzed reaction was voltammetrically detected. Peroxidase activity could be quantified using the steady-state current on the voltammogram after subtracting the blank and using the

This twenty-four item scale assesses students' actual and desired political-social activism in terms of physical participation, communication activities, and information-gathering activities. About ten minutes are required to complete the instrument. The scale is divided into two subscales. The first twelve items (ACT-A) question respondents on…

New Ru(III) isothiosemicarbazone complexes [RuCl(EPh3)L(1-4)] (E=P or As) were obtained from the reactions between [RuCl3(EPh3)3] and bis(salicylaldehyde)-S-methylisothiosemicarbazone (H2L(1-3))/bis(2-hydroxy-naphthaldehyde)-S-methylisothiosemicarbazone (H2L(4)) ligands. The new complexes were characterized by using elemental analyses and various spectral (UV-Vis, IR, (1)H NMR, FAB-Mass and EPR) methods. The redox properties of the complexes were studied by using cyclic voltammetric method. The new complexes were subjected to various biological investigations such as antioxidant assays involving DPPH radical, hydroxyl radical, nitric oxide radical and hydrogen peroxide, DNA/protein interaction studies and in vitro cytotoxic studies against human breast cancer cell line (MCF-7). New complexes showed excellent free radicals scavenging ability and could bind with DNA via intercalation. Protein binding studies using fluorescence spectroscopy showed that the new complexes could bind strongly with bovine serum albumin (BSA). Photo cleavage experiments using DNA of E-coli bacterium exhibited the DNA cleavage ability of the complexes. Further, the in vitro anticancer activity studies on the new complexes against MCF-7 cell line exhibited the ability of Ru(III) isothiosemicarbazone complexes to suppress the development of malignant neoplastic disease cells. PMID:24911273

We analyze self-propelling organisms, or active particles, in a periodic asymmetric potential. Unlike standard ratchet effect for Brownian particles requiring external forcing, in the case of active particles asymmetric potential alone produces a net drift speed (active ratchet effect). By using theoretical models and numerical simulations we demonstrate the emergence of the rectification process in the presence of an asymmetric piecewise periodic potential. The broken spatial symmetry (external potential) and time symmetry (active particles) are sufficient ingredients to sustain unidirectional transport. Our findings open the way to new mechanisms to move in directional manner motile organisms by using external periodic static fields.

Ternary oxovanadium(IV) complexes [VO(salmdtc)(B)] (1-3), where salmdtc is dianionic N-salicylidene-S-methyldithiocarbazate and B is N,N-donor phenanthroline bases like 1,10-phenanthroline (phen, 1), dipyrido[3,2-d:2',3'-f]quinoxaline (dpq, 2) and dipyrido[3,2-a:2',3'-c]phenazine (dppz, 3), are prepared, characterized and their DNA binding and DNA cleavage activity studied. Complex 3 is structurally characterized by single-crystal X-ray crystallography. The molecular structure shows the presence of a vanadyl group in six-coordinate VN(3)O(2)S coordination geometry. The S-methyldithiocarbazate Schiff base acts as a tridentate NSO-donor ligand in a meridional binding mode. The N,N-donor heterocyclic base displays a chelating mode of binding with an N-donor site trans to the vanadyl oxo-group. The complexes show a d-d band in the range of 675-707 nm in DMF. They exhibit an irreversible oxidative cyclic voltammetric response near 0.9 V due to the V(V)/V(IV) couple and a quasi-reversible reductive V(IV)/V(III) redox couple near -1.0 V vs. SCE in DMF-0.1M TBAP. The complexes show good binding propensity to calf thymus DNA giving binding constant values in the range of 7.4 x 10(4)-2.3 x 10(5)M(-1). The thermal denaturation and viscosity binding data suggest DNA surface and/or groove binding nature of the complexes. The complexes show poor chemical nuclease activity in dark in the presence of 3-mercaptopropionic acid (MPA) or hydrogen peroxide. The dpq and dppz complexes show efficient DNA cleavage activity in UV-A light of 365 nm via a type-II mechanistic pathway involving formation of singlet oxygen ((1)O(2)) as the reactive species. PMID:18279964

Blending scholarship and activism, whether domestic or international, takes some real work. Two scholar-activists reflect on why and how activism can be more than academic labor in this feature of the "Academe" journal. This feature includes the following brief reflections on political work, both local and global that demonstrates how on campus…

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A catalyst activator particularly adapted for use in the activation of metal complexes of metals of Group 3-10 for polymerization of ethylenically unsaturated polymerizable monomers, especially olefins, comprising two Group 13 metal or metalloid atoms and a ligand structure including at least one bridging group connecting ligands on the two Group 13 metal or metalloid atoms.

Twenty-four activities suitable for outdoor use by elementary school children are outlined. Activities designed to make children aware of their environment include soil painting, burr collecting, insect and pond water collecting, studies of insect galls and field mice, succession studies, and a model of natural selection using dyed toothpicks. A…

This document consists of activities and references for teaching astronomy. The activities (which include objectives, list of materials needed, and procedures) focus on: observing the Big Dipper and locating the North Star; examining the Big Dipper's stars; making and using an astrolabe; examining retograde motion of Mars; measuring the Sun's…

Two-phase nanocomposite layers based on porous silicon and nonstoichiometric tin oxide were fabricated by various methods. The structure, as well as elemental and phase composition, of the obtained nanocomposites were studied using transmission and scanning electron microscopy, Raman spectroscopy, Auger electron spectroscopy, and X-ray photoelectron spectroscopy. The results obtained confirm the formation of nanocomposite layers with a thickness as large as 2 {mu}m thick and SnO{sub x} stoichiometry coefficients x = 1.0-2.0. Significant tin diffusion into the porous silicon matrix with D{sub eff} Almost-Equal-To 10{sup -14} cm{sup 2} s{sup -1} was observed upon annealing at 770 K. Test sensor structures based on por-Si/SnO{sub x} nanocomposite layers grown by magnetron deposition showed fairly high stability of properties and sensitivity to NO{sub 2}.

Two-photon stereolithography is used for rapid prototyping of submicrometre molecularly imprinted polymer-based 3D structures. The structures are evaluated as chemical sensing elements and their specific recognition properties for target molecules are confirmed. The 3D design capability is exploited and highlighted through the fabrication of an all-organic molecularly imprinted polymeric microelectromechanical sensor. PMID:27145145

There has been an urgent need for an effective and efficient upper limb rehabilitation method for poststroke patients. We present a Micro-Sensor-based Upper Limb rehabilitation System for poststroke patients. The wearable motion capture units are attached to upper limb segments embedded in the fabric of garments. The body segment orientation…

This work presents the use of nanoporous anodic aluminium oxide [AAO] for reflective interferometric sensing of volatile sulphur compounds and hydrogen sulphide [H2S] gas. Detection is based on changes of the interference signal from AAO porous layer as a result of specific adsorption of gas molecules with sulphur functional groups on a gold-coated surface. A nanoporous AAO sensing platform with optimised pore diameters (30 nm) and length (4 µm) was fabricated using a two-step anodization process in 0.3 M oxalic, followed by coating with a thin gold film (8 nm). The AAO is assembled in a specially designed microfluidic chip supported with a miniature fibre optic system that is able to measure changes of reflective interference signal (Fabry-Perrot fringes). When the sensor is exposed to a small concentration of H2S gas, the interference signal showed a concentration-dependent wavelength shifting of the Fabry-Perot interference fringe spectrum, as a result of the adsorption of H2S molecules on the Au surface and changes in the refractive index of the AAO. A practical biomedical application of reflectometric interference spectroscopy [RIfS] Au-AAO sensor for malodour measurement was successfully shown. The RIfS method based on a nanoporous AAO platform is simple, easy to miniaturise, inexpensive and has great potential for development of gas sensing devices for a range of medical and environmental applications. PMID:22176687

Health diagnostics is an area where major improvements have been identified for potential implementation into the design of new reusable launch vehicles in order to reduce life cycle costs, to increase safety margins, and to improve mission reliability. NASA Ames is leading the effort to develop inspection and health management technologies for thermal protection systems. This paper summarizes a joint project between NASA Ames and SRI International to develop 'SensorTags,' radio frequency identification devices coupled with event-recording sensors, that can be embedded in the thermal protection system to monitor temperature or other quantities of interest. Two prototype SensorTag designs containing thermal fuses to indicate a temperature overlimit are presented and discussed.

This paper describes the development of NH4+- sensitive membranes based on various polymer materials incorporating nonactine as the ionophore for long-term performance CHEMFETs. Different composition of membranes based on plasticized PVC, carboxylated PVC, plasticized PVC modified by decylmethacrylate, polysiloxane and Siloprene were studied. Although polysiloxane membrane presented the most improved adhesion to the chip surface, the Siloprene membrane was successfully applied to design durable NH4+-sensitive CHEMFETs. These sensors showed NH4+-responses with good selectivity even after 14 months of continuous exposure to conditioning electrolyte.

We present a method based on an electrochemical sensor array and a back propagation artificial neural network for detection and quantification of four properties of lubrication oil, namely water (0, 500 ppm, 1000 ppm), total acid number (TAN) (13.1, 13.7, 14.4, 15.6 mg KOH g‑1), soot (0, 1%, 2%, 3%) and sulfur content (1.3%, 1.37%, 1.44%, 1.51%). The sensor array, consisting of four micromachined electrochemical sensors, detects the four properties with overlapping sensitivities. A total set of 36 oil samples containing mixtures of water, soot, and sulfuric acid with different concentrations were prepared for testing. The sensor array’s responses were then divided to three sets: training sets (80% data), validation sets (10%) and testing sets (10%). Several back propagation artificial neural network architectures were trained with the training and validation sets; one architecture with four input neurons, 50 and 5 neurons in the first and second hidden layer, and four neurons in the output layer was selected. The selected neural network was then tested using the four sets of testing data (10%). Test results demonstrated that the developed artificial neural network is able to quantitatively determine the four lubrication properties (water, TAN, soot, and sulfur content) with a maximum prediction error of 18.8%, 6.0%, 6.7%, and 5.4%, respectively, indicting a good match between the target and predicted values. With the developed network, the sensor array could be potentially used for online lubricant oil condition monitoring.

A zeolite-fiber integrated chemical sensor was developed for in situ point detection of chemical warfare agents. The sensor was made by fine-polishing the MFI polycrystalline zeolite thin film synthesized on the endface of the single mode optical fiber. The sensor device operates by measuring the optical thickness changes of the zeolite thin film caused by the adsorption of analytes into the zeolite channels. The sensor was demonstrated for sensitive detection of toluene and dimethyl methylphosphonate (DMMP).

Vanadium oxide, manganese oxide, tungsten oxide, and nickel oxide nanowires were investigated for their applicability as chemiresistive gas sensors. Nanowires have excellent surface-to-volume ratios which yield higher sensitivities than bulk materials. Sensing elements consisting of these materials were assembled in an array to create an electronic nose platform. Dielectrophoresis was used to position the nanomaterials onto a microfabricated array of electrodes, which was subsequently mounted onto a leadless chip carrier and printed circuit board for rapid testing. Samples were tested in an enclosed chamber with vapors of acetone, isopropanol, methanol, and aqueous ammonia. The change in resistance of each assembly was measured. Responses varied between nanowire compositions, each demonstrating unique and repeatable responses to different gases; this enabled direct detection of the gases from the ensemble response. Sensitivities were calculated based on the fractional resistance change in a saturated environment and ranged from 6 × 10-4 to 2 × 10-5%change ppm-1.

Health diagnostics is an area where major improvements have been identified for potential implementation into the design of new reusable launch vehicles in order to reduce life cycle costs, to increase safety margins, and to improve mission reliability. NASA Ames is leading the effort to develop inspection and health management technologies for thermal protection systems. This paper summarizes a joint project between NASA Ames and SRI International to develop SensorTags, radio-frequency identification devices coupled with event-recording sensors, that can be embedded in the thermal protection system to monitor temperature or other quantities of interest. Two prototype SensorTag designs containing thermal fuses to indicate a temperature overlimit are presented and discussed.

The molecular binding between the glutamine binding-protein (GlnBP) from Escherichia coli and L-glutamine (Gln) is detected by means of an optical biosensor based on porous silicon technology. The binding event is optically transduced in the wavelength shift of the porous silicon optical microcavity (PSMC) reflectivity spectrum. The hydrophobic interaction links the GlnBP, which acts as a molecular probe for Gln, to the hydrogenated porous silicon surface area. We can thus avoid any preliminary surface functionalization process. The protein infiltrated PSMC results stable to oxidation at least for few cycles of wet measurements. The penetration of the proteins into the pores of the porous silicon matrix has been optimized: a strong base post-etch process increases the pore size and removes any nanostructure on top and inside the porous silicon multilayer while does not degrade the optical response and the quality of the microcavity.

The rapid autonomous detection of pathogenic microorganisms and bioagents by field deployable platforms is critical to human health and safety. To achieve a high level of sensitivity for fluidic detection applications, we have developed a 330 MHz Love wave acoustic biosensor on 36{sup o} YX Lithium Tantalate (LTO). Each die has four delay-line detection channels, permitting simultaneous measurement of multiple analytes or for parallel detection of single analyte containing samples. Crucial to our biosensor was the development of a transducer that excites the shear horizontal (SH) mode, through optimization of the transducer, minimizing propagation losses and reducing undesirable modes. Detection was achieved by comparing the reference phase of an input signal to the phase shift from the biosensor using an integrated electronic multi-readout system connected to a laptop computer or PDA. The Love wave acoustic arrays were centered at 330 MHz, shifting to 325-328 MHz after application of the silicon dioxide waveguides. The insertion loss was -6 dB with an out-of-band rejection of 35 dB. The amplitude and phase ripple were 2.5 dB p-p and 2-3{sup o} p-p, respectively. Time-domain gating confirmed propagation of the SH mode while showing suppression of the triple transit. Antigen capture and mass detection experiments demonstrate a sensitivity of 7.19 {+-} 0.74{sup o} mm{sup 2}/ng with a detection limit of 6.7 {+-} 0.40 pg/mm{sup 2} for each channel.

We have further developed and demonstrated the novel ORNL micro-calorimetric spectroscopy technique for the detections and characterization of toxic organic substances. In this technique target molecules were allowed to adsorb on the surface of sub-femtojoule sensitive micromechanical thermal detectors. The adsorption of molecules on the thermal detector surface causes a differential surface stress resulting in an initial ''trigger''. By exposing the thermal detector microstructure elements to different photon wavelengths, an extremely sensitive and unique photothermal signature response was obtained. We adsorbed sub-monolayer levels of target chemicals onto the bi-material detector surfaces. We obtained infrared photothermal spectra for trace concentrations of several organics such as diisopropyl methylphosphonate (DIMP), and trinitrotoluene (TNT) over the wavelength region 2.5 to 14.5 {micro}m. We found that in the wavelength region 2.5 to 14.5 {micro}m the photothermal spectra of DIMP and TNT exhibit a number of peaks and are in excellent agreement with traditional infrared absorption spectra found in the literature. Chemical detectors based on micro-calorimetric spectroscopy can be used to sensitively sense a relatively small number of molecules adsorbed on a thermal detector surface. This photothermal signature resulting from photon irradiation and subsequent thermal transfer can be used for improved chemical characterization.

Important factors in the application of chemical sensing technology to space applications are low mass, small size, and low power. All of these attributes are enabled by the application of MEMS and micro-fabrication technology to chemical sensing. Several Sandia projects that apply these technologies to the development of new chemical sensing capabilities with the potential for space applications will be described. The Polychromator project is a joint project with Honeywell and MIT to develop an electrically programmable diffraction grating that can be programmed to synthesize the spectra of molecules. This grating will be used as the reference cell in a gas correlation radiometer to enable remote chemical detection of most chemical species. Another area of research where micro-fabrication is having a large impact is the development of a lab on a chip. Sandia's efforts to develop the {mu}ChemLab{trademark} will be described including the development of microfabricated pre-concentrators, chromatographic columns, and detectors. Chemical sensors are evolving in the direction of sensor arrays with pattern recognition methods applied to interpret the pattern of response. Sandia's development of micro-fabricated chemiresistor arrays and the VERI pattern recognition technology to interpret the sensor response will be described.

Routine determination of trace metals in complex media is still a difficult task for many analytical instruments. The aim of this work was to compare three electro-chemical instruments [a standard potentiostat (Autolab), a commercially available miniaturized potentiostat (PalmSens) and a homemade micropotentiostat] for easy-to-use and sensitive determination of cadmium(II) and lead(II) ions. The lowest detection limits (hundreds of pM) for both metals was achieved by using of the standard potentiostat, followed by the miniaturized potentiostat (tens of nM) and the homemade instrument (hundreds of nM). Nevertheless, all potentiostats were sensitive enough to evaluate contamination of the environment, because the environmental limits for both metals are higher than detection limits of the instruments. Further, we tested all used potentiostats and working electrodes on analysis of environmental samples (rainwater, flour and plant extract) with artificially added cadmium(II) and lead(II). Based on the similar results obtained for all potentiostats we choose a homemade instrument with a carbon tip working electrode for our subsequent environmental experiments, in which we analyzed maize and sunflower seedlings and rainwater obtained from various sites in the Czech Republic. PMID:22219663

The most commonly used methods for the preparation of sensing film of micro-gas sensors are physical methods such as r.f. sputtering, thermal evaporation, spary pyrolysis and CVD. Though it is somewhat difficult to be compatible with microelectronic processes, the chemical preparation method such as sol-gel method has many advantages over the physical ones like additive incorporation and surface control. In this experiment, the authors have prepared tin oxide thin film by sol-gel method combined with spin-coating. The compatibility of the film process to the microelectronic process and CO gas sensing characteristics of the fabricated film have been investigated.

Electromagnetic (EM) tracking systems have been successfully used for Surgical Navigation in ENT, cranial, and spine applications for several years. Catheter sized micro EM sensors have also been used in tightly controlled cardiac mapping and pulmonary applications. EM systems have the benefit over optical navigation systems of not requiring a line-of-sight between devices. Ferrous metals or conductive materials that are transient within the EM working volume may impact tracking performance. Effective methods for detecting and reporting EM field distortions are generally well known. Distortion compensation can be achieved for objects that have a static spatial relationship to a tracking sensor. New commercially available micro EM tracking systems offer opportunities for expanded image-guided navigation procedures. It is important to know and understand how well these systems perform with different surgical tables and ancillary equipment. By their design and intended use, micro EM sensors will be located at the distal tip of tracked devices and therefore be in closer proximity to the tables. Our goal was to define a simple and portable process that could be used to estimate the EM tracker accuracy, and to vet a large number of popular general surgery and imaging tables that are used in the United States and abroad.

In this work, we theoretically and experimentally investigate the thermal response of whispering gallery mode microresonators operating in an aqueous glycerol medium. Thermal stabilisation of the resonance wavelength is realised by appropriate choice of the resonator radius and glycerol concentration, with a 60 fold reduction in thermal sensitivity demonstrated. Finally, we employ our stabilised system to determine the thermal dependence of the molecular polarisability of adsorbed bovine serum albumin molecules and the refractive index of dextran and poly(diallyldimethylammonium chloride) coatings.

This report provides a summary of the three-year LDRD (Laboratory Directed Research and Development) project aimed at developing microchemical sensors for continuous, in-situ monitoring of volatile organic compounds. A chemiresistor sensor array was integrated with a unique, waterproof housing that allows the sensors to be operated in a variety of media including air, soil, and water. Numerous tests were performed to evaluate and improve the sensitivity, stability, and discriminatory capabilities of the chemiresistors. Field tests were conducted in California, Nevada, and New Mexico to further test and develop the sensors in actual environments within integrated monitoring systems. The field tests addressed issues regarding data acquisition, telemetry, power requirements, data processing, and other engineering requirements. Significant advances were made in the areas of polymer optimization, packaging, data analysis, discrimination, design, and information dissemination (e.g., real-time web posting of data; see www.sandia.gov/sensor). This project has stimulated significant interest among commercial and academic institutions. A CRADA (Cooperative Research and Development Agreement) was initiated in FY03 to investigate manufacturing methods, and a Work for Others contract was established between Sandia and Edwards Air Force Base for FY02-FY04. Funding was also obtained from DOE as part of their Advanced Monitoring Systems Initiative program from FY01 to FY03, and a DOE EMSP contract was awarded jointly to Sandia and INEEL for FY04-FY06. Contracts were also established for collaborative research with Brigham Young University to further evaluate, understand, and improve the performance of the chemiresistor sensors.

This paper describes the design, fabrication and characterization of a flow sensor for high-temperature, or otherwise aggressive, environments, like, e.g. the propulsion system of a small spacecraft. The sensor was fabricated using 8 mol% yttria stabilized zirconia (YSZ8) high-temperature co-fired ceramic (HTCC) tape and screen printed platinum paste. A calorimetric flow sensor design was used, with five 80 µm wide conductors, separated by 160 µm, in a 0.4 mm wide, 0.1 mm deep and 12.5 mm long flow channel. The central conductor was used as a heater for the sensor, and the two adjacent conductors were used to resistively measure the heat transferred from the heater by forced convection. The two outermost conductors were used to study the influence of an auxiliary heat source on the sensor. The resistances of the sensor conductors were measured using four-point connections, as the gas flow rate was slowly increased from 0 to 40 sccm, with different power supplied through the central heater, as well as with an upstream or downstream heater powered. In this study, the thermal and electrical integrability of microcomponents on the YSZ8 substrate was of particular interest and, hence, the influence of thermal and ionic conduction in the substrate was studied in detail. The effect of the ion conductivity of YSZ8 was studied by measuring the resistance of a platinum conductor and the resistance between two adjacent conductors on YSZ8, in a furnace at temperatures from 20 to 930 °C and by measuring the resistance with increasing current through a conductor. With this design, the influence of ion conductivity through the substrate became apparent above 700 °C. The sensitivity of the sensor was up to 1 mΩ sccm-1 in a range of 0-10 sccm. The results show that the signal from the sensor is influenced by the integrated auxiliary heating conductors and that these auxiliary heaters provide a way to balance disturbing heat sources, e.g. thrusters or other electronics, in conjunction with the flow sensor.

Nanocrystalline porous silicon films (nanodots) and polymeric silicon wires (nanowires) have been used to detect chemicals in gas and liquid phase. Transduction mechanisms using quantum confinement derived photoluminescence and optical reflectivity have been used. Photoluminescence intensity is modulated by energy or electron transfer induced quenching, and a shift of the Fabry-Perot reflectivity fringes from thin nanocrystalline films occurs upon molecular absorption. Examples of irreversible detection and reversible sensing modes for explosives, nerve warfare agents, and various odors of commercial interest will be provided. A catalyst can be incorporated into the nanomaterials to provide specificity for the analyte of interest.

Metal oxide semiconductor gas sensors with modulated working temperature should reveal small thermal time constant in comparison to the time constants of chemical reactions between gas atmosphere and sensitive layer. In such case analyzed sensor response is dominated with specific phenomena originated from these reactions. A way the sensors are mounted has big influence on the sensor thermal time constants. In experiments authors used gas sensors with ceramic and micromachined silicon substrates glued to the case or suspended on thin wires. Although mechanical stability and durability of glued sensors are better, the lower power consumption and lower time constants are possible with sensors mounted using thin wires.

A widespread need exists for portable, real-time, in-situ chemical, physical, and radiological sensors in characterization of mixed waste, groundwater, contaminated soils and process streams. None of the currently available technologies offer a clear path to the development of se...

An array of chemically-sensitive field-effect transistors (CHEMFETs) that measure both work function and bulk resistance changes in thin films was used to detect volatile organic compounds. Carbon black/organic polymer composite films were deposited onto the CHEMFETs using an automated microdispensing method.

This volume contains 16 chapters on the application of activation analysis in the fields of life sciences, biological materials, coal and its effluents, environmental samples, archaeology, material science, and forensics. Each chapter is processed separately for the data base.

Integrin-mediated cell adhesion is important for development, immune responses, hemostasis and wound healing. Integrins also function as signal transducing receptors that can control intracellular pathways that regulate cell survival, proliferation, and cell fate. Conversely, cells can modulate the affinity of integrins for their ligands a process operationally defined as integrin activation. Analysis of activation of integrins has now provided a detailed molecular understanding of this unique form of “inside-out” signal transduction and revealed new paradigms of how transmembrane domains (TMD) can transmit long range allosteric changes in transmembrane proteins. Here, we will review how talin and mediates integrin activation and how the integrin TMD can transmit these inside out signals. [BMB Reports 2014; 47(12): 655-659] PMID:25388208

Four series of azidopurines have been synthesized and tested for cytokinin activity in the tobacco callus bioassay: 2- and 8-azido-N6-benzyladenines, -N6-(Δ2-isopentenyl)adenines, and -zeatins, and N6-(2- and 4-azidobenzyl)adenines. The compounds having 2-azido substitution on the adenine ring are as active as the corresponding parent compounds, while those with 8-azido substitution are about 10 or more times as active. The 8-azidozeatin, which is the most active cytokinin observed, exhibited higher than minimal detectable activity at 1.2 × 10−5 micromolar, the lowest concentration tested. The shape of the growth curve indicates that even a concentration as low as 5 × 10−6 micromolar would probably be effective. By comparison, the lowest active concentration ever reported for zeatin has been 5 × 10−5 micromolar, representing a sensitivity rarely attained. All of the azido compounds have been submitted to photolysis in aqueous ethanol, and the photoproducts have been detected and identified by low and high resolution mass spectrometry. They are rationalized as products of abstraction and insertion reactions of the intermediate nitrenes. The potential of the major released products as cytokinins was also assessed by bioassay. 2-Azido-N6-(Δ2-isopentenyl)adenine competed with [14C]kinetin for the cytokinin-binding protein isolated from wheat germ. When the azido compound was photolysed in the presence of this protein, its attachment effectively blocked the binding of [14C]kinetin. PMID:16661017

... Lifting small weights – you can even use bottled water or cans of food as weights Watch these videos for muscle strengthening exercises to do at home or at the gym. If you do muscle-strengthening activities with weights, check out the do’s and don’ ...

Presents a flow chart for naming inorganic compounds. Although it is not necessary for students to memorize rules, preliminary skills needed before using the chart are outlined. Also presents an activity in which the mass of an imaginary atom is determined using lead shot, Petri dishes, and a platform balance. (JN)

This report is aimed to show the author's activities to support the LDRD. The title is 'Investigation of the Double-C Behavior in the Pu-Ga Time-Temperature-Transformation Diagram' The sections are: (1) Sample Holder Test; (2) Calculation of x-ray diffraction patterns; (3) Literature search and preparing publications; (4) Tasks Required for APS Experiments; and (5) Communications.

The liver performs a vital role in metabolism, secretion, storage, and detoxification of endogenous and exogenous substances. Oxidative stress and free radicals enhance the severity of hepatic damage, which can be overcome by the antioxidant mechanism. Plant extracts can be the best source of such antioxidants and mediate hepatoprotective activity. In this chapter, high-dose paracetamol-induced hepatotoxicity in rat model is discussed with explanations of biochemical and histopathological studies. PMID:26939279

Analgesics are agents which selectively relieve pain by acting in the CNS and peripheral pain mediators without changing consciousness. Analgesics may be narcotic or non-narcotic. The study of pain in animals raises ethical, philosophical, and technical problems. Both peripheral and central pain models are included to make the test more evident for the analgesic property of the plant. This chapter highlights methods such as hot plate and formalin and acetic acid-induced pain models to check the analgesic activity of medicinal plants. PMID:26939272

An active sonar system is one in which pulses of acoustic energy are launched into the water for the purpose of producing echoes. By examining the echoes of transmitted pulses, it affords the capability of both detecting the presence of and estimating the range, and in certain cases, the bearing, of an underwater target. In its most common arrangement, the transmitter (or projector) and the receiver are colocated. This is known as the monostatic configuration and is depicted in Figure 1. When this is not so, it is known as a bistatic or multistatic configuration.

There have been many reviews concerned with antimicrobial food packaging, and with the use of antifungal compounds, but none provided an exhaustive picture of the applications of active packaging to control fungal spoilage. Very recently, many studies have been done in these fields, therefore it is timely to review this topic. This article examines the effects of essential oils, preservatives, natural products, chemical fungicides, nanoparticles coated to different films, and chitosan in vitro on the growth of moulds, but also in vivo on the mould free shelf-life of bread, cheese, and fresh fruits and vegetables. A short section is also dedicated to yeasts. All the applications are described from a microbiological point of view, and these were sorted depending on the name of the species. Methods and results obtained are discussed. Essential oils and preservatives were ranked by increased efficacy on mould growth. For all the tested molecules, Penicillium species were shown more sensitive than Aspergillus species. However, comparison between the results was difficult because it appeared that the efficiency of active packaging depended greatly on the environmental factors of food such as water activity, pH, temperature, NaCl concentration, the nature, the size, and the mode of application of the films, in addition to the fact that the amount of released antifungal compounds was not constant with time. PMID:26803804

This study is part of a series of Studies in Geophysics that have been undertaken for the Geophysics Research Forum by the Geophysics Study Committee. One purpose of each study is to provide assessments from the scientific community to aid policymakers in decisions on societal problems that involve geophysics. An important part of such assessments is an evaluation of the adequacy of current geophysical knowledge and the appropriateness of current research programs as a source of information required for those decisions. The study addresses our current scientific understanding of active tectonics --- particularly the patterns and rates of ongoing tectonic processes. Many of these processes cannot be described reasonably using the limited instrumental or historical records; however, most can be described adequately for practical purposes using the geologic record of the past 500,000 years. A program of fundamental research focusing especially on Quaternary tectonic geology and geomorphology, paleoseismology, neotectonics, and geodesy is recommended to better understand ongoing, active tectonic processes. This volume contains 16 papers. Individual papers are indexed separately on the Energy Database.

The oxidation pathways of methanol (MeOH) have been the subject of intense research due to its possible application as a liquid fuel in polyelectrolyte membrane (PEM) fuel cells. The design of improved catalysts for MeOH oxidation requires a deep understanding of these complex oxidation pathways. This paper will provide a discussion of the literature concerning the extensive research carried out in acidic and alkaline electrolytes. It will highlight techniques that have proven useful in the determination of product ratios, analysis of surface poisoning, anion adsorption, and oxide formation processes, in addition to the effects of temperature on the MeOH oxidation pathways at bulk polycrystalline platinum (Pt(poly)) electrodes. This discussion will provide a framework with which to begin the analysis of activation energy (E(a)) values. This kinetic parameter may prove useful in characterizing the rate-limiting step of the MeOH oxidation at an electrode surface. This paper will present a procedure for the determination of E(a) values for MeOH oxidation at a Pt(poly) electrode in acidic and alkaline media. Values from 24-76 kJ mol(-1) in acidic media and from 36-86 kJ mol(-1) in alkaline media were calculated and found to be a function of applied potential and direction of the potential sweep in a voltammetric experiment. Factors that influence the magnitude of the calculated E(a) include surface poisoning from MeOH oxidation intermediates, anion adsorption from the electrolyte, pH effects, and oxide formation processes. These factors are all potential, and temperature, dependent and must clearly be addressed when citing E(a) values in the literature. Comparison of E(a) values must be between systems of comparable electrochemical environment and at the same potential. E(a) values obtained on bulk Pt(poly), compared with other catalysts, may give insight into the superiority of other Pt-based catalysts for MeOH oxidation and lead to the development of new catalysts

DAVIC (Digital Audio Visual Council) is the defacto standardization organization established in Mar. 1994, based on international consensus for digital audio visual services. After completion of MPEG2 standardization, the broadcasting industry, the communication industry, the computer industry, and consumer electronics industry have started development of concrete services and products. Especially the interactive digital audio visual services, such as Video On Demand (VOD) or Near Video On Demand (NVOD), have become hot topics all over the world. Such interactive digital audio visual services are combined technologies of multi-media coding, digital transmission and computer networking. Therefore more than 150 organizations from all industry sectors have participated in DAVIC and are contributing from their own industrial contexts. DAVIC's basic policy is to use the available technologies specified by the other standards bodies as much as possible. So DAVIC's standardization activities have close relationship with ISO IEC/JTC1/SC29, ITU-T SG 9, ATM-Forum, IETF, IMA, DVB, etc. DAVIC is trying to specify Applications, Reference Models, Security, Usage Information Control, and the interfaces and protocols among the Content Provider, the Server, the core network, the access network, and the Set Top Unit. DAVIC's first goal is to specify DAVIC1.0 based on CFP1 (Call for Proposal) and CFP2 by Dec. 1995, and the next direction is under preparation for further progress based on CFP3 and CFP4.

The present report is an update on activities for the second year of funding. Research leading to a detailed characterization of antiproton annihilation in nuclei has resulted in a published analysis of fast deuteron production from carbon and uranium targets. This follows previously reported work and publications by our group on gamma-ray, neutral and charged pion, proton, and neutron production. The deuteron measurements are important to our SHIVA Star antiproton- catalyzed microfission experiment at the Phillips Laboratory, Kirtland AFB, in that they help constrain theoretical models of light nuclei production and subsequent energy deposition in the target. Work continues at SHIVA Star on working fluid formation and target compression for the microfission experiment. Excellent progress has been made, both theoretically and experimentally, on these important aspects of the experiment. The Penn State group, working in collaboration with Los Alamos National Laboratory physicists, trapped and held up to 721,000 antiprotons per beam injection pulse from the LEAR accelerator during July, 1993. This was a crucial step to the ultimate goal of transferring large numbers of antiprotons to the Phillips Laboratory for the antiproton-catalyzed microfission experiment.

The human visual system observes and understands a scene/image by making a series of fixations. Every fixation point lies inside a particular region of arbitrary shape and size in the scene which can either be an object or just a part of it. We define as a basic segmentation problem the task of segmenting that region containing the fixation point. Segmenting the region containing the fixation is equivalent to finding the enclosing contour- a connected set of boundary edge fragments in the edge map of the scene - around the fixation. This enclosing contour should be a depth boundary. We present here a novel algorithm that finds this bounding contour and achieves the segmentation of one object, given the fixation. The proposed segmentation framework combines monocular cues (color/intensity/texture) with stereo and/or motion, in a cue independent manner. The semantic robots of the immediate future will be able to use this algorithm to automatically find objects in any environment. The capability of automatically segmenting objects in their visual field can bring the visual processing to the next level. Our approach is different from current approaches. While existing work attempts to segment the whole scene at once into many areas, we segment only one image region, specifically the one containing the fixation point. Experiments with real imagery collected by our active robot and from the known databases 1 demonstrate the promise of the approach. PMID:20686671

It’s well known, astronomy in Uzbekistan has ancient roots and traditions (e.g., Mirzo Ulugh Beg, Abū al-Rayhān al-Bīrūnī, Abū ‘Abdallāh al-Khwārizmī) and astronomical heritage carefully preserved. Nowadays uzbek astronomers play a key role in scientific research but also in OAD and Decadal Plan activity in the Central Asia region. International Aerospace School (IASS) is an amazing and wonderful event held annually about 30 years. IASS is unique project in the region, and at the beginning we spent the Summer and Winter Schools. At present in the summer camp we gather about 50 teenage and undergraduate students over the country and abroad (France, Malaysia, Turkey, Azerbaijan, Pakistan, Russia, etc.). They are selected on the basis of tests of astronomy and space issues. During two weeks of IASS camp the invited scientists, cosmonauts and astronauts as well as other specialists give lectures and engage in practical exercises with IASS students in astronomy, including daily observations of the Sun and night sky observations with meniscus telescope, space research and exploration, aerospace modelling, preparation and presentation of original projects. This is important that IASS gives not theoretical grounds only but also practically train the students and the hands-on training is the major aims of IASS. Lectures and practice in the field of astronomy carried out with the direct involvement and generous assistance of Uranoscope Association (Paris, France). The current 26-th IASS is planned to held in July 2015.

Teaming is so common in today's project management environment that most of us assume it comes naturally. We further assume that when presented with meaningful and challenging work, project teams will naturally engage in productive activity to complete their tasks. This assumption is expressed in the simple (but false) equation: Team + Work = Teamwork. Although this equation appears simple and straightforward, it is far from true for most project organizations whose reality is a complex web of institutional norms based on individual achievement and rewards. This is illustrated by the very first successful team experience from my early Air Force career. As a young lieutenant, I was sent to Squadron Officer School, which was the first in the series of Air Force professional military education courses I was required to complete during my career. We were immediately formed into teams of twelve officers. Much of the course featured competition between these teams. As the most junior member of my team, I quickly observed the tremendous pressure to show individual leadership capability. At one point early in the course, almost everyone in our group was vying to become the team leader. This conflict was so intense that it caused us to fail miserably in our first outdoor team building exercise. We spent so much time fighting over leadership that we were unable to complete any of the events on the outdoor obstacle course. This complete lack of success was so disheartening to me that I gave our team little hope for future success. What followed was a very intense period of bickering, conflict, and even shouting matches as our dysfunctional team tried to cope with our early failures and find some way to succeed. British physician and researcher Wilfred Bion (Experiences in Groups, 1961) discovered that there are powerful psychological forces inherent in all groups that divert from accomplishing their primary tasks. To overcome these restraining forces and use the potential

Femtomolar (fM) leveled lead ions were electrochemically detected using a bucky-gel coated glassy carbon electrode and differential pulse anodic stripping voltammetry. The bucky-gel was composed of dithizone, ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate), and multi-walled carbon nanotubes (MWCNTs). The fabrication of the bucky-gel coated electrode was optimized. The modified electrode was characterized with voltammetry, electrochemical impedance spectroscopy, and chronoamperometry. After the accumulation of lead ions into the bucky-gel modified electrode at -1.2V vs. saturated calomel electrode (SCE) for 5 min in a pH 4.4 sodium acetate-acetate acid buffer solution, differential pulse anodic stripping voltammograms of the accumulated lead show an anodic wave at -0.58 V. The anodic peak current is detectable for lead ions in the concentration range from 1.0 μM down to 500 fM. The detection limit is calculated to be 100 fM. The proposed method was successfully applied for the detection of lead ions in lake water. PMID:20875583

A proof of concept for the label-free detection of bacteriophage MS2, a model indicator of microbiological contamination, is validated in this work as a porous silicon (pSi) membrane-based electrochemical biosensor. PSi membranes were used to afford nanochannel architectures. The sensing mechanism was based on the nanochannel blockage caused by MS2 binding to immobilized capture antibodies. This blockage was quantified by measuring the oxidation current of the electroactive species reaching the electrode surface, by means of differential pulse voltammetry (DPV). The immunosensor showed a limit of detection of 6 pfu/mL in buffer, allowing the detection of MS2 to levels commonly found in real-world applications, and proved to be unaffected by matrix effects when analyzing MS2 in reservoir water. This platform enables the straightforward, direct and sensitive detection of a broad range of target analytes and constitutes a promising approach towards the development of portable electronic point of sample analysis devices. PMID:26803413

The electrochemical performances of hydrogen- and oxygen-terminated nano-crystalline diamond film electrodes were investigated by cyclic voltammetry and AC impedance spectroscopy. In addition, the surface morphologies, phase structures, and chemical states of the two diamond films were analysed by scanning probe microscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy, respectively. The results indicated that the potential window is narrower for the hydrogen-terminated nano-crystalline diamond film than for the oxygen-terminated one. The diamond film resistance and capacitance of oxygen-terminated diamond film are much larger than those of the hydrogen-terminated diamond film, and the polarization resistances and double-layer capacitance corresponding to oxygen-terminated diamond film are both one order of magnitude larger than those corresponding to the hydrogen-terminated diamond film. The electrochemical behaviours of the two diamond film electrodes are discussed.

A novel electrochemical immunosensor has been developed to detect phosphorylated proteins, phospho-p53(15) and phospho-p53(392), simultaneously. Different apoferritin templated metal phosphates were used as distinguishable signal reporters (apoferritin templated cadmium phosphates (ATCP) and apoferritin templated lead phosphates (ATLP)) to enhance the detection sensitivity. Here, magnetic Fe3O4 nanoparticles functionalized phospho-p53(15) capture antibody (MP-p53(15)c-Ab) and phospho-p53(392) capture antibody (MP-p53(392)c-Ab), respectively, were used to specifically capture phospho-p53(15) and phospho-p53(392) antigens, followed by immunorecognition with p53(15) detection antibody (p53(15)d-Ab) and p53(392) detection antibody (p53(392)d-Ab) to form sandwich-like immunocomplexes. SiO2@Au nanocomposites served as nanocarriers for co-immobilization of both d-Ab and signal reporters (ATCP/SiO2@Au/p53(15)d-Ab, ATLP/SiO2@Au/p53(392)d-Ab), which greatly amplified the detection signal. The distinguished current responses were achieved by electrochemical detection of cadmium ions and lead ions with square wave voltammetry (SWV) after dissolution with acid. The proposed immunoassay exhibited high sensitivity and selectivity for the detection of phospho-p53(15) and phospho-p53(392) simultaneously. The linear relationships between electrochemical responses and the concentrations of phospho-p53(15) and phospho-p53(392) were obtained in the range of 0.1-20ng/mL and 0.05-20ng/mL, respectively. The detection limits were 0.05 and 0.02ng/mL (S/N=3), respectively. This strategy provides a new platform for simultaneous immunoassay of multiple protein biomarkers. PMID:26844908

Results are presented on determinations of reduction potentials and their temperature dependence of selected ions in diopsidic melt, by using linear sweep voltammetry. Diffusion coefficients were measured for cations of Eu, Mn, Cr, and In. Enthalpies and entropies of reduction were determined for the cations V(V), Cr(3+), Mn(2+), Mn(3+), Fe(2+), Cu(2+), Mo(VI), Sn(IV), and Eu(3+). Reduction potentials were used to study the structural state of cations in the melt.

We demonstrate low-voltage electrowetting at the surface of freshly cleaved highly oriented pyrolytic graphite (HOPG). Using cyclic voltammetry (CV), electrowetting of a droplet of a sodium perchlorate solution is observed at moderately positive potentials on high-quality (low step edge coverage) HOPG, leading to significant changes in the contact angle and relative contact diameter that are comparable to the results of the widely studied electrowetting on dielectric (EWOD) system, but over a much lower voltage range. The electrowetting behavior is found to be reasonably fast, reversible, and repeatable for at least 20 cyclic scans (maximum tested). In contrast to classical electrowetting, e.g., EWOD, the electrowetting of the droplet on HOPG occurs with the intercalation/deintercalation of anions between the graphene layers of graphite, driven by the applied potential, observed in the CV response, and detected by X-ray photoelectron spectroscopy. The electrowetting behavior is strongly influenced by those factors that affect the extent of the intercalation/deintercalation of ions on graphite, such as potential range scan rate, potential polarity, quality of the HOPG substrate (step edge density and step height), and type of anion in the solution. In addition to perchlorate, sulfate salts also promote electrowetting, but some other salts do not. Our findings suggest a new mechanism for electrowetting based on ion intercalation, and the results are important to fundamental electrochemistry as well as to diversifying the means by which electrowetting can be controlled and applied. PMID:27406680

ABSTRACT A method is reported for the determination of diphenylamine and butylated hydroxytoluene in mineral and synthetic oil. The procedure used differential pulse voltammetry with a glassy carbon electrode. This method was then used for determining these antioxidants in supporting electrolyte consisting of dilute sulfuric acid and sodium dodecyl sulfonate in ethanol. Anodic peaks were obtained for both analytes. Oxidation peaks at 250 mV were observed from a mixture of butylated hydroxytoluene and dinonyl diphenylamine, allowing their simultaneous determination. This approach was successfully used for the determination of dinonyl diphenylamine and butylated hydroxytoluene in fortified mineral and synthetic oils with good accuracy and precision. PMID:27365537

Cyclic voltammetry is a widely used and powerful tool for sensitively and selectively measuring hydrogen peroxide (H2O2). Herein, voltammetry was combined with electron paramagnetic resonance spectroscopy to identify and define the role of an oxygen-centered radical liberated during the oxidation of H2O2. The spin-trap reagents, 5,5-dimethyl-1-pyrroline N-oxide (DMPO) and 2-ethoxycarbonyl-2-methyl-3,4-dihydro-2H-pyrrole-1-oxide (EMPO), were employed. Spectra exhibit distinct hyperfine patterns that clearly identify the DMPO(•)-OH and EMPO(•)-OH adducts. Multiple linear regression analysis of voltammograms demonstrated that the hydroxyl radical is a principal contributor to the voltammetry of H2O2, as signal is attenuated when this species is trapped. These data incorporate a missing, fundamental element to our knowledge of the mechanisms that underlie H2O2 electrochemistry. PMID:26840154

The electrochemical behaviour of desloratadine (DLOR) and its derivative 3-hydroxydesloratadine (3OH-DLOR) was investigated by direct current (DCP) polarography, cyclic (CV), differential pulse (DPV) and square-wave (SWV) voltammetry in Britton-Robinson (BR) buffer solutions (pH 4-11). Both compounds are reduced at mercury electrode in irreversible two electron reduction of the C=N bond of the pyridine ring in their molecules. The difference in their electrochemical behaviour was investigated, and the most pronounced distinction is observed at pH > 9, as a consequence of the deprotonation of the phenolic moiety in 3OH-DLOR molecule, yielding significant change in their reduction potentials (Ep DLOR = -1.48 V, and Ep 3OH-DLOR = -1.6 V). The observed results correlate with calculated LUMO energy levels and Hammet substituent constants (σ). Based on the difference in the reduction potential for DLOR and 3OH-DLOR, conditions for simultaneous determination these two molecules in alkaline medium were established. The best selectivity was achieved using SWV method at pH 10. The linearity of the calibration graphs were achieved in the concentration range from 1.5 × 10-6 M - 1 × 10-5 M for DLOR and 7.5 × 10-6 M - 5 × 10-5 M for 3OH-DLOR with detection limits of 2.29 × 10-7 M and 2.08 × 10-6 M, and determination limits of 7.64 × 10-7 M and 6.94 × 10-6 M, for DLOR and 3OH-DLOR, respectively. The method was checked in human plasma sample. Good response was obtained with LOD and LOQ values of 4.63 × 10-7 M and 1.54 × 10-6 M, for DLOR and 2.39 × 10-6 M and 7.97 × 10-6 M, 3OH-DLOR, respectively. PMID:24061817

We have developed a novel bacterial detection technique by desiccating a bacterial suspension deposited on an electrode. It was also found that the use of an indium-tin-oxide (ITO) electrode dramatically improved the resolution of the voltammogram, allowing us to observe two pairs of redox peaks, each assigned to the adsorption of isoprenoid ubiquinone (UQn) and menaquinone (MKn), which were present in the bacterial cell envelopes, giving midpeak potentials of -0.015 and -0.25 V versus Ag|AgCl|saturated KCl| at pH 7.0, respectively. Most of the microorganisms classified in both the Gram-negative and -positive bacteria gave well-defined redox peaks, demonstrating that this procedure made the detection of the quinones possible without solvent extraction. It has been demonstrated that the present technique can be used not only for the detection of bacteria, but also for profiling of the isoprenoid quinones, which play important roles in electron and proton transfer in microorganisms. In this respect, the present technique provides a much more straightforward way than the solvent extraction in that one sample can be prepared in 1 min by heat evaporation of a suspension containing the targeted bacteria, which has been applied on the ITO electrode. PMID:26218886

A novel electrochemical sensing approach, based on electropolymerization of a molecularly imprinted polypyrrole (MIPpy) film onto a glassy carbon electrode (GCE) surface, was developed for the detection of flunixin (FXN). The sensing conditions and the performance of the constructed sensor were assessed by cyclic, differential pulse and (DPV) square wave voltammetry (SWV). The sensor exhibited high sensitivity, with linear responses in the range of 5.0 to 50.0 µM with detection limits of 1.5 and 1.0 µM for DPV and SWV, respectively. In addition, the sensor showed high selectivity towards FXN in comparison to other interferents. The sensor was successfully utilized for the direct determination of FXN in buffalo raw milk samples. PMID:27242945

In this study, a carbon paste electrode modified with TiO2 nanoparticles and ferrocene monocarboxylic acid (FM) was used to prepare a novel electrochemical sensor. The objective of this novel electrode modification was to seek new electrochemical performances for the detection of methyldopa in the presence of folic acid and glycine. The peak potentials recorded in a phosphate buffer solution (PBS) of pH7.0 were 325, 750 and 880 mV vs. Ag/AgCl/KCl (3.0M) for methyldopa, folic acid and glycine, respectively. Under the optimum pH of 7.0, the oxidation of methyldopa occurred at a potential about 160 mV less positive than that of the unmodified carbon paste electrode (CPE). The response of catalytic current with methyldopa concentration showed a linear relation in the range from 2.0×10(-7) to 1.0×10(-4)M with a detection limit of 8.0 (± 0.2)×10(-8)M. PMID:24433900

Oxidation of phenol on platinum electrodes rapidly leads to the formation of a passivating film on the surface of these electrodes. Studies of cyclic voltammetry and chronoamperometry combined with high-performance liquid chromatography (HPLC) analyses have shown that the presence of carbon black avoids these phenomena of passivation and thus allows the complete mineralization of phenol. The nature of carbon black and the pH value are two important factors which are studied here. VULCAN XC-72 R, an intrinsic p-type semiconductor, having a large specific area, showed all its efficiency when cyclic voltammetry experiments were carried out in an acid medium (pH 2.2). HPLC analyses revealed the appearance of several by-products such as hydroquinone and benzoquinone, and maleic and fumaric acids.

Electrical stimulation of the nigrostriatal pathway released dopamine (DA) in the striatum of the anaesthetized rat. The level of DA released by 10-s stimulus trains was measured by high-speed cyclic voltammetry. Metoclopramide (10 mg/kg) increased DA release by approximately 20%. Apomorphine (1.76 mg/kg) caused a approximately 40% decrease in release which was blocked by metoclopramide. Ascorbate (1.76 g/kg) had no effect on stimulated DA release. Furthermore, pretreatment of rats with ascorbate trebled the striatal extracellular ascorbate level, but failed to modify the effects of metoclopramide and apomorphine on DA release. We conclude that ascorbate has no effect on the presynaptic autoreceptors that modulate striatal DA release in vivo. PMID:2999651

An improvement of selectivity for electrochemical detection of dopamine (DA) with differential pulse voltammetry is achieved by covalently modifying a glassy carbon electrode (GCE) with O-carboxymethylchitosan (OCMCS). The amphiphilic chitosan provides electrostatic accumulation of DA onto the electrode surface. In a phosphate buffer solution (pH 6.0), a pair of well-defined reversible redox waves of DA was observed at the OCMCS/GCE with a ΔEp of 52 mV. The anodic peak current obtained from the differential pulse voltammetry of dopamine was linearly dependent on its concentration in the range of 6.0 × 10-8 to 7.0 × 10-6 M, with a correlation coefficient of 0.998. The detection limit (S/N = 3) was found to be 1.5 × 10-9 M. The modified electrode had been applied to the determination of DA in human serum samples with satisfactory results.

Voltammetry of partially oxidized porous molybdenum alkali metal thermoelectric converter (AMTEC) electrodes from about 600 to 1000 K revealed a series of redox processes within the AMTEC operational voltage range which can be used to establish the electronic and ionic conductivities of these electrodes. Improved estimates of the free energies of formation of Na2Mo3O6, NaMoO2, and Na3MoO4 are obtained. Evidence is provided for the slow corrosive attack by Na2MoO4 on molybdenum. The ionic conductivity of Na2MoO4 is found to be sufficiently large at temperatures of greater than 700 K to explain the observed electrochemical phenomena in addition to the enhanced sodium transport in AMTEC electrodes below the freezing point of Na2MoO4.

A well derivative reduction wave of methaqualone (MTQ) was obtained in 0.033 mol dm(-3) B-R (pH 3.76) buffer solution by single-sweep oscillopolarography. The peak potential is -1.36 V (vs. saturated calomel reference electrode, SCE). The peak current is proportional to the concentration of methaqualone over the range of 7.0 x 10(-8)-9.0 x 10(-6) mol dm(-3). The method has been successfully applied to the determination of methaqualone in tablets. The wave is believed to result from irreversible adsorption through studies of its electrochemical behavior and reaction mechanism. PMID:18968991

A new graphene/zinc oxide nanorods modified glassy carbon electrode (GR/ZnORs/GCE) based electrochemical sensor has been developed for the sensitive determination tizanidine (TZ) in solubilized system. The fabricated sensor was characterized by various electrochemical methods. Different kinetic parameters affecting the monitored electrocatalytic response were investigated and optimized for tizanidine determination at fabricated GR/ZnORs/GCE sensor and successfully compared with the results obtained at GR/SiO2/GCE, GR/GCE and at bare GCE. Under optimized conditions the square wave current is linear over the concentration range 0.80 ng mL-1 to 10.0 μg mL-1 with detection limit and quantification limit of 0.10 ng mL-1 and 3.45 ng mL-1 respectively. The applicability of proposed method is further extended to in vitro determination of the drug in pharmaceutical formulation with an acceptable recovery from 97.89% to 101.09%.

The human amyloid beta (Aβ) peptides, Aβ1-40 and Aβ1-42, structural modifications, from soluble monomers to fully formed fibrils through intermediate structures, were investigated, and the results were compared with those obtained for the inverse Aβ40-1 and Aβ42-1, mutant Aβ1-40Phe(10) and Aβ1-40Nle(35), and rat Aβ1-40Rat peptide sequences. The aggregation was followed at a slow rate, in chloride free media and room temperature, and revealed to be a sequence-structure process, dependent on the physicochemical properties of each Aβ peptide isoforms, and occurring at different rates and by different pathways. The fibrilization process was investigated by atomic force microscopy (AFM), via changes in the adsorption morphology from: (i) initially random coiled structures of ∼0.6 nm height, corresponding to the Aβ peptide monomers in random coil or in α-helix conformations, to (ii) aggregates and protofibrils of 1.5-6.0 nm height and (iii) two types of fibrils, corresponding to the Aβ peptide in a β-sheet configuration. The reactivity of the carbon electrode surface was considered. The hydrophobic surface induced rapid changes of the Aβ peptide conformations, and differences between the adsorbed fibrils, formed at the carbon surface (beaded, thin, <2.0 nm height) or in solution (long, smooth, thick, >2.0 nm height), were detected. Differential pulse voltammetry showed that, according to their primary structure, the Aβ peptides undergo oxidation in one or two steps, the first step corresponding to the tyrosine amino acids oxidation, and the second one to the histidine and methionine amino acids oxidation. The fibrilization process was electrochemically detected via the decrease of the Aβ peptide oxidation peak currents that occurred in a time dependent manner. PMID:27216391

A novel, sensitive immunochromatographic electrochemical biosensor (IEB) which combines an immunochromatographic strip technique with an electrochemical detection technique is demonstrated. The IEB takes advantages of the speed and low-cost of the conventional immunochromatographic test kits and high-sensitivity of stripping voltammetry. Bismuth ions (Bi3+) have been coupled with the antibody through the bifunctional chelating agent diethylenetriamine pentaacetic acid (DTPA). After immunoreactions, Bi3+ was released and quantified by anodic stripping voltammetry at a built-in single-use screen-printed electrode. As an example for the applications of such novel device, the detection of human chorionic gonadotronphin (HCG) in a specimen was performed. This biosensor provides a more user-friendly, rapid, clinically accurate, and less expensive immunoassay for such analysis in specimens than currently available test kits.

Aqueous metal behavior is strongly regulated by speciation, which in turn is highly dependent on complexation. Trace metal complexation is difficult to characterize in dynamically changing systems due to a lack of analytical methods that can rapidly report free-metal concentrations. In this paper, we perform proof-of-principle experiments that demonstrate the utility of fast-scan cyclic voltammetry (FSCV) for providing speciation information in real-time by characterizing dynamic Cu(II) binding. We study Cu(II) FSCV responses in 3-(N-morpholino)propanesulfonic acid (MOPS) buffer and characterize the hydrodynamic aspects of our experimental setup (continuously stirred tank reactor). We observe Cu(II) complexation in real-time using five ligands with differing formation constants of Cu(II) complexation. Finally, we utilize geochemical models to fit our real-time experimental Cu(II)-binding curves. Our proof-of-principle experiments show that FSCV is a powerful tool for studying real-time Cu(II) complexation, which is essential speciation information for better interpretation of Cu(II) behavior in dynamically changing systems, such as those encountered in biology or the environment. PMID:27322355

A glassy carbon electrode modified with a Nafion/MWCNTs composite is shown to enable the determination of codeine using differential pulse voltammetry in phosphate buffer of pH 3.0. At a preconcentration time of 15 s, the calibration graph is linear in the 0.5 µM (0.15 mg·L−1) to 15 µM (4.5 mg·L−1) concentration range with a correlation coefficient of 0.998. The detection limit at a preconcentration time of 120 s is as low as 4.5 μg·L−1. The repeatability of the method at a 0.6 μg·L−1 concentration level, expressed as the RSD, is 3.7% (for n = 5). The method was successfully applied and validated by analyzing codeine in drug, human plasma, and urine samples. PMID:25741451

Until recently, there had been two conflicting views about the order of copper oxides (Cu(2)O and CuO) in their cathodic reduction with a neutral or weak alkaline electrolyte (typically 0.1 M KCl). In 2001, we successfully employed a strongly alkaline electrolyte (SAE; i.e., 6 M KOH + 1 M LiOH) to achieve a perfect separation of the reduction peaks of the two oxides. It was then found that the oxides were reduced in SAE according to a thermodynamic order, i.e., "CuO → Cu(2)O", and also that the reduction of CuO occurred in one step. At an extremely slow scan rate of <0.2 mV s(-1), however, CuO appears to be reduced in two steps via Cu(2)O. It has also been shown that the developed method with SAE can be applied to analysis of various corrosion products, including Cu(2)S, Cu(OH)(2), and patinas. Use of the developed method has allowed researchers to clarify the mechanism of the atmospheric corrosion of copper. PMID:22498457

A composite obtained by depositing platinum nanoparticles in a polytyramine (PTy) matrix, electrochemically formed on graphite substrate, was used as electrode material for the investigation of phenol oxidation by use of anodic voltammetry. The results show that, in acidic media, the measurement of the oxidation peak current can be used as the basis for a simple, rapid method for the determination of phenol within a concentration range of 0.3-10 mM. A much better resistance to fouling during phenol detection (compared both with smooth platinum and with Pt nanoparticles on bare graphite substrate) is the main advantage of the Pt-PTy composite. These results are also noteworthy because they provide a basis for additional experiments devoted to obtaining new composite materials with improved performances for phenol anodic oxidation. PMID:20462693

... fitness. Your fitness routine should include aerobic and strength-training activities, and may also include stretching activities. Aerobic ... Examples include walking, jogging, bicycling, swimming, and tennis. Strength-training activities These activities increase the strength and endurance ...

A miniature wireless implantable electrochemical glucose system for continuous glucose monitoring with good selectivity, sensitivity, linearity and long term stability was developed. First, highly sensitive, long-term stable and reusable planar H2O2 microelectrodes have been fabricated by microlithography. These electrodes composed of a 300 nm Pt black layer situated on a 5 um thick Au layer, provide effective protection to the underlying chromium adhesion layer. Using repeated cyclic voltammetric sweeps in flowing buffer solution, highly sensitive Pt black working electrodes were realized with five-decade linear dynamic range and low detection limit (10 nM) for H2O2 at low oxidation potentials. Second, a highly sensitive, low cost and flexible microwire biosensor was described using 25-mum thick gold wire as working electrode together with 125-mum thick Pt/Ir and Ag wires as counter and reference electrode, embedded within a PDMS-filled polyethylene tube. Surface area and activity of sensor was enhanced by converting gold electrode to nanoporous configuration followed by electrodeposition of platinum black. Glucose oxidase based biosensors by electrodeposition of poly(o-phenylenediamine) and glucose oxidase on the working electrode, displayed a higher glucose sensitivity (1.2 mA mM-1 cm-2) than highest literature reported. In addition it exhibits wide detection range (up to 20 mM) and selectivity (>95%). Third, novel miniaturized and flexible microelectrode arrays with 8 of 25 mum electrodes displayed the much needed 3D diffusion profiles similar to a single 25 mum microelectrode, but with one order increase in current levels. These microelectrode arrays displayed a H2O2 sensitivity of 13 mA mM-1 cm-2, a wide dynamic range of 100 nM to 10 mM, limit of detection of 10 nM. These microwire based edge plane microsensors incorporated flexibility, miniaturization and low operation potential are an promising approach for continuous in vivo metabolic monitoring. Fourth

The benefits of doing adapted physical exercise for elderly people have been proven. For more than thirty years, the French Federation for an Active Retirement has been striving to help people age well by proposing multiple activities to remain in good health after the age of 50. Doctors, activity leaders and federal instructors are attentive to each individual's capacities. PMID:27449307

Integrates contemporary theories of learning into a theory of learning as activity. Explains ecological psychology, changes in understanding of learning, activity systems and activity theory (including the integration of consciousness and activity), and activity structure; and discusses learning as a cognitive and social process. (LRW)